dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
time_units
large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-1ab555f16b654ade937dccaeb6cb5b60
Cc1cc(C)c(-c2c3nc(c(-c4ccc(C(C)(C)C)cc4)c4ccc([nH]4)c(C4OCC(C)(C)CO4)c4nc(c(-c5ccc(C(C)(C)C)cc5)c5ccc2[nH]5)C=C4)C=C3)c(C)c1>>Cc1cc(C)c(-c2c3nc(c(-c4ccc(C(C)(C)C)cc4)c4ccc([nH]4)c(C=O)c4nc(c(-c5ccc(C(C)(C)C)cc5)c5ccc2[nH]5)C=C4)C=C3)c(C)c1
C(C)(C)(C)C1=CC=C(C=C1)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C4OCC(CO4)(C)C)N3)C3=CC=C(C=C3)C(C)(C)C)=N2)C2=C(C=C(C=C2C)C)C.C(=O)(C(F)(F)F)O.O>>C(C)(C)(C)C1=CC=C(C=C1)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C=O)N3)C3=CC=C(C=C3)C(C)(C)C)=N2)C2=C(C=C(C=C2C)C)C
CC1(C)CO[CH:28]([c:27]2[c:25]3[cH:24][cH:23][c:22]([c:11](-[c:12]4[cH:13][cH:14][c:15]([C:16]([CH3:17])([CH3:18])[CH3:19])[cH:20][cH:21]4)[c:10]4[n:9][c:8]([c:7](-[c:6]5[c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:55][c:53]5[CH3:54])[c:47]5[cH:46][cH:45][c:44]([c:33](-[c:34]6[cH:35][cH:36][c:37]([C:38]([CH3:39])([CH3:40])[CH3...
Cc1cc(C)c(-c2c3nc(c(-c4ccc(C(C)(C)C)cc4)c4ccc([nH]4)c(C4OCC(C)(C)CO4)c4nc(c(-c5ccc(C(C)(C)C)cc5)c5ccc2[nH]5)C=C4)C=C3)c(C)c1
Cc1cc(C)c(-c2c3nc(c(-c4ccc(C(C)(C)C)cc4)c4ccc([nH]4)c(C=O)c4nc(c(-c5ccc(C(C)(C)C)cc5)c5ccc2[nH]5)C=C4)C=C3)c(C)c1
null
null
C(Cl)Cl
Miscellaneous
Acetal hydrolysis to aldehyde
c0e8259a4c04433c939fe17907d7eafe1c52bcb535318030bf0e1cb6f82c0712
84d5a69453aa750f462aa94a6bf2116fc17c5d88a9619aaa9eefb74b0c09848d
C1=Cc2nc1cc1ccc([nH]1)c(-c1ccccc1)c1nc(c(-c3ccccc3)c3ccc([nH]3)c2-c2ccccc2)C=C1
C-C1(-C)-C-O-[CH;D3;+0:1](-[c:2](:[c:3](:[c:4]):[#7;a:5]:[c:6]):[c:7]2:[#7;a:8]:[c:9]-[C:10]=[C:11]-2)-[O;H0;D2;+0:12]-C-1>>[O;H0;D1;+0:12]=[CH;D2;+0:1]-[c:2](:[c:3](:[c:4]):[#7;a:5]:[c:6]):[c:7]1:[#7;a:8]:[c:9]-[C:10]=[C:11]-1
96.5
[{"value": 92.0, "product": "C(C)(C)(C)C1=CC=C(C=C1)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C=O)N3)C3=CC=C(C=C3)C(C)(C)C)=N2)C2=C(C=C(C=C2C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.5, "product": "C(C)(C)(C)C1=CC=C(C=C1)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C=O)N3)C3=CC=C(C=C...
null
null
2.5
HOUR
Following a general procedure,22 a solution of 4 (43 mg, 0.05 mmol) in CH2Cl2 (5 mL) was treated with TFA/water (0.5 mL, 1:1) to give a biphasic solution. After stirring at room temperature for 2.5 h, CH2Cl2 was added. The organic layer was washed (saturated aqueous NaHCO3 and brine), dried (Na2SO4), concentrated, and ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Aldehyde
C1COCOC1
null
c1ccccc1.c1ccccc1.c1ccccc1.C1=Cc2cc3ccc(cc4nc(cc5ccc(cc1n2)n5)C=C4)n3
HO-
C(Cl)Cl
null
2.5
Cc1cc(C)c(-c2c3nc(c(-c4ccc(C(C)(C)C)cc4)c4ccc([nH]4)c(C4OCC(C)(C)CO4)c4nc(c(-c5ccc(C(C)(C)C)cc5)c5ccc2[nH]5)C=C4)C=C3)c(C)c1>C(Cl)Cl>Cc1cc(C)c(-c2c3nc(c(-c4ccc(C(C)(C)C)cc4)c4ccc([nH]4)c(C=O)c4nc(c(-c5ccc(C(C)(C)C)cc5)c5ccc2[nH]5)C=C4)C=C3)c(C)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ac1066e2a00a46a68a42da26e6ac36ce
CC(C)(CO)CO.O=CC(=O)O>>CC1(C)COC(C(=O)O)OC1
O.C(C=O)(=O)O.CC(CO)(CO)C>>C(=O)(O)C1OCC(CO1)(C)C
[CH3:1][C:2]([CH3:3])([CH2:4][OH:5])[CH2:11][OH:10].O=[CH:6][C:7](=[O:8])[OH:9]>>[CH3:1][C:2]1([CH3:3])[CH2:4][O:5][CH:6]([C:7](=[O:8])[OH:9])[O:10][CH2:11]1
CC(C)(CO)CO.O=CC(=O)O
CC1(C)COC(C(=O)O)OC1
null
null
C1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
09991f411aacffcc904d1b314d4846ed4bc3fcd70ecd0a878cedf349d9162730
7ac65b5a5f576337ce8e86e0130eb9b4757ca21b2419a0e82bbdfd5def30ee73
C1COCOC1
O=[CH;D2;+0:1]-[C:2](=[O;D1;H0:3])-[O;D1;H1:4].[OH;D1;+0:5]-[C:6]-[C:7]-[C:8]-[OH;D1;+0:9]>>[O;D1;H0:3]=[C:2](-[O;D1;H1:4])-[CH;D3;+0:1]1-[O;H0;D2;+0:5]-[C:6]-[C:7]-[C:8]-[O;H0;D2;+0:9]-1
73.4
[{"value": 73.0, "product": "C(=O)(O)C1OCC(CO1)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73.4, "product": "C(=O)(O)C1OCC(CO1)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Following a general procedure,23 a mixture of glyoxylic acid monohydrate (5.0 g, 54 mmol), 2,2-dimethyl 1,3-propanediol (8.5 g, 81 mmol) and Amberlyst-15 ion-exchange resin (100 mg) in benzene (140 mL) was refluxed for 15 h in a flask fitted with a Dean-Stark apparatus. The reaction mixture was filtered. The filtrate w...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary alcohol.Primary alcohol
Ether.Ether
null
C1COCOC1
C1COCOC1
HO-
C1=CC=CC=C1
null
null
CC(C)(CO)CO.O=CC(=O)O>C1=CC=CC=C1>CC1(C)COC(C(=O)O)OC1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-de88f6777451494bbb26cbe1ef4f25d6
CC1(C)COC(c2c3nc(c(-c4ccccc4)c4ccc([nH]4)c(C4OCC(C)(C)CO4)c4nc(c(-c5ccccc5)c5ccc2[nH]5)C=C4)C=C3)OC1>>O=Cc1c2nc(c(-c3ccccc3)c3ccc([nH]3)c(C=O)c3nc(c(-c4ccccc4)c4ccc1[nH]4)C=C3)C=C2
C(Cl)Cl.C(C)(=O)OCC.CC1(COC(OC1)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C4=CC=CC=C4)N3)C3OCC(CO3)(C)C)=N2)C2=CC=CC=C2)C.C(=O)(C(F)(F)F)O.O>>C(=O)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C4=CC=CC=C4)N3)C=O)=N2)C2=CC=CC=C2
CC1(C)CO[CH:2]([c:3]2[c:4]3[n:5][c:6]([c:7](-[c:8]4[cH:9][cH:10][cH:11][cH:12][cH:13]4)[c:14]4[cH:15][cH:16][c:17]([nH:18]4)[c:19]([CH:20]4OCC(C)(C)C[O:21]4)[c:22]4[n:23][c:24]([c:25](-[c:26]5[cH:27][cH:28][cH:29][cH:30][cH:31]5)[c:32]5[cH:33][cH:34][c:35]2[nH:36]5)[CH:37]=[CH:38]4)[CH:39]=[CH:40]3)[O:1]C1>>[O:1]=[CH:2...
CC1(C)COC(c2c3nc(c(-c4ccccc4)c4ccc([nH]4)c(C4OCC(C)(C)CO4)c4nc(c(-c5ccccc5)c5ccc2[nH]5)C=C4)C=C3)OC1
O=Cc1c2nc(c(-c3ccccc3)c3ccc([nH]3)c(C=O)c3nc(c(-c4ccccc4)c4ccc1[nH]4)C=C3)C=C2
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
25afb5e990cc694e9d051666ccb4295610f2a73c81de017ecb8368b0c5bb9111
e21cb1bdfd69a4be8a457a57bfa9f8563cedb23c177c9d451a21afc104d55beb
C1=Cc2nc1cc1ccc([nH]1)c(-c1ccccc1)c1nc(cc3ccc([nH]3)c2-c2ccccc2)C=C1
C-C1(-C)-C-O-[CH;D3;+0:1](-[c:2](:[c:3](:[c:4]):[#7;a:5]:[c:6]):[c:7]2:[#7;a:8]:[c:9]-[C:10]=[C:11]-2)-[O;H0;D2;+0:12]-C-1.C-C1(-C)-C-O-[CH;D3;+0:13](-[c:14](:[c:15](:[c:16]):[#7;a:17]:[c:18]):[c:19]2:[#7;a:20]:[c:21]-[C:22]=[C:23]-2)-[O;H0;D2;+0:24]-C-1>>[O;H0;D1;+0:12]=[CH;D2;+0:1]-[c:2](:[c:3](:[c:4]):[#7;a:5]:[c:6]...
83
[{"value": 83.0, "product": "C(=O)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C4=CC=CC=C4)N3)C=O)=N2)C2=CC=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.0, "product": "C(=O)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C4=CC=CC=C4)N3)C=O)=N2)C2=CC=CC=C2", "details": "CALCULATEDPERCENTYIELD...
null
null
3
DAY
As described for 5, a solution of 14 (30 mg, 44 μmol) in CH2Cl2 (5.0 mL) was treated with TFA/water (2.0 mL, 1:1) with stirring at room temperature for 3 days. Standard workup including chromatography (silica, CH2Cl2/ethyl acetate) gave a purple green solid (18.7 mg, 83%): IR (neat) 1673, 1550, 1120 cm−1; 1H NMR δ −2.3...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Ether
Aldehyde.Aldehyde
C1COCOC1.C1COCOC1
null
c1ccccc1.c1ccccc1.C1=Cc2cc3ccc(cc4nc(cc5ccc(cc1n2)n5)C=C4)n3
HO-
C(Cl)Cl
null
72
CC1(C)COC(c2c3nc(c(-c4ccccc4)c4ccc([nH]4)c(C4OCC(C)(C)CO4)c4nc(c(-c5ccccc5)c5ccc2[nH]5)C=C4)C=C3)OC1>C(Cl)Cl>O=Cc1c2nc(c(-c3ccccc3)c3ccc([nH]3)c(C=O)c3nc(c(-c4ccccc4)c4ccc1[nH]4)C=C3)C=C2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-0986f615c1f044319bcf86fa07aa69f1
CC1(C)COC(c2c3nc(c(C4OCC(C)(C)CO4)c4ccc([nH]4)c(-c4ccccc4)c4nc(c(-c5ccccc5)c5ccc2[nH]5)C=C4)C=C3)OC1>>O=Cc1c2nc(c(C=O)c3ccc([nH]3)c(-c3ccccc3)c3nc(c(-c4ccccc4)c4ccc1[nH]4)C=C3)C=C2
CC1(COC(OC1)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C4OCC(CO4)(C)C)N3)C3=CC=CC=C3)=N2)C2=CC=CC=C2)C.C(=O)(C(F)(F)F)O.O>>C(=O)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C=O)N3)C3=CC=CC=C3)=N2)C2=CC=CC=C2
CC1(C)CO[CH:2]([c:3]2[c:4]3[n:5][c:6]([c:7]([CH:8]4OCC(C)(C)C[O:9]4)[c:10]4[cH:11][cH:12][c:13]([nH:14]4)[c:15](-[c:16]4[cH:17][cH:18][cH:19][cH:20][cH:21]4)[c:22]4[n:23][c:24]([c:25](-[c:26]5[cH:27][cH:28][cH:29][cH:30][cH:31]5)[c:32]5[cH:33][cH:34][c:35]2[nH:36]5)[CH:37]=[CH:38]4)[CH:39]=[CH:40]3)[O:1]C1>>[O:1]=[CH:2...
CC1(C)COC(c2c3nc(c(C4OCC(C)(C)CO4)c4ccc([nH]4)c(-c4ccccc4)c4nc(c(-c5ccccc5)c5ccc2[nH]5)C=C4)C=C3)OC1
O=Cc1c2nc(c(C=O)c3ccc([nH]3)c(-c3ccccc3)c3nc(c(-c4ccccc4)c4ccc1[nH]4)C=C3)C=C2
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
25afb5e990cc694e9d051666ccb4295610f2a73c81de017ecb8368b0c5bb9111
e21cb1bdfd69a4be8a457a57bfa9f8563cedb23c177c9d451a21afc104d55beb
C1=Cc2cc3ccc([nH]3)c(-c3ccccc3)c3nc(c(-c4ccccc4)c4ccc(cc1n2)[nH]4)C=C3
C-C1(-C)-C-O-[CH;D3;+0:1](-[c:2](:[c:3](:[c:4]):[#7;a:5]:[c:6]):[c:7]2:[#7;a:8]:[c:9](:[c:10](-[CH;D3;+0:11]3-O-C-C(-C)(-C)-C-[O;H0;D2;+0:12]-3):[c:13](:[c:14]):[#7;a:15]:[c:16])-[C:17]=[C:18]-2)-[O;H0;D2;+0:19]-C-1>>[O;H0;D1;+0:19]=[CH;D2;+0:1]-[c:2](:[c:3](:[c:4]):[#7;a:5]:[c:6]):[c:7]1:[#7;a:8]:[c:9](:[c:10](-[CH;D2...
88
[{"value": 88.0, "product": "C(=O)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C=O)N3)C3=CC=CC=C3)=N2)C2=CC=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.8, "product": "C(=O)C=1C2=CC=C(N2)C(=C2C=CC(C(=C3C=CC(=C(C=4C=CC1N4)C=O)N3)C3=CC=CC=C3)=N2)C2=CC=CC=C2", "details": "CALCULATEDPERCENTYIELD...
null
null
null
null
As described for 5, a solution of 17 (30 mg, 44 μmol) in CH2Cl2 (5.0 mL) was treated with TFA/water (2.0 mL, 1:1) at room temperature for 3 days. The standard workup including chromatography (silica, CHCl3/hexanes) afforded a purple solid (19.8 mg, 88%): IR (neat) 1672, 1548, 1166 cm−1; 1H NMR δ −2.19 (s, 2H), 7.76-7.8...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Ether
Aldehyde.Aldehyde
C1COCOC1.C1COCOC1
null
c1ccccc1.c1ccccc1.C1=Cc2cc3ccc(cc4nc(cc5ccc(cc1n2)n5)C=C4)n3
HO-
C(Cl)Cl
null
null
CC1(C)COC(c2c3nc(c(C4OCC(C)(C)CO4)c4ccc([nH]4)c(-c4ccccc4)c4nc(c(-c5ccccc5)c5ccc2[nH]5)C=C4)C=C3)OC1>C(Cl)Cl>O=Cc1c2nc(c(C=O)c3ccc([nH]3)c(-c3ccccc3)c3nc(c(-c4ccccc4)c4ccc1[nH]4)C=C3)C=C2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3f464347dcc84cd7a0f1603cd8663c97
CCCCC=O.O=C1C=CCC1>>CCCCC(O)C1=CCCC1=O
C1(C=CCC1)=O.C(CCCC)=O.C(CCC)P(CCCC)CCCC>>OC(CCCC)C=1C(CCC1)=O
[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]=[O:6].[CH:7]1=[CH:8][CH2:9][CH2:10][C:11]1=[O:12]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]([OH:6])[C:7]1=[CH:8][CH2:9][CH2:10][C:11]1=[O:12]
CCCCC=O.O=C1C=CCC1
CCCCC(O)C1=CCCC1=O
null
null
C1CCOC1
C-C Coupling
OtherReaction
d982483ca196073df722bce8466788858afd4e2743b087e877ba8e9bd813efc2
7d7139092067ff475e8e8a4ad6adb4833600ca969e282ed08dc56c016dccb864
O=C1C=CCC1
[C:1]-[C:2]-[CH;D2;+0:3]=[O;H0;D1;+0:4].[O;D1;H0:5]=[C:6]1-[C:7]-[C:8]-[C:9]=[CH;D2;+0:10]-1>>[C:1]-[C:2]-[CH;D3;+0:3](-[OH;D1;+0:4])-[C;H0;D3;+0:10]1=[C:9]-[C:8]-[C:7]-[C:6]-1=[O;D1;H0:5]
92
[{"value": 92.0, "product": "OC(CCCC)C=1C(CCC1)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of cyclopentenone (1.23 g, 15 mmol), pentanal (1.94 g, 22.5 mmol), rac-1,1′-bi-2-naphthol (429 mg, 1.5 mmol) and tributyl phosphine (606 mg, 3 mmol) in dry THF (12 ml) was stirred at 20° C. under Argon for 3 hours. The solution was then passed through a short column of SiO2 (cyclohexane/Et2O 6:4) to obtain t...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone.Secondary alcohol
C1=CCCC1
C1=CCCC1
C1=CCCC1
null
C1CCOC1
null
null
CCCCC=O.O=C1C=CCC1>C1CCOC1>CCCCC(O)C1=CCCC1=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-157c9ed3dcb14c5a90079d5afbbf6d01
CC(C)(C)C(=O)O.CC(C)(C)C([O-])([O-])[O-].CCCCC(O)C1=CCCC1=O>>CCCCC=C1C(=O)CCC1CC(=O)OC
OC(CCCC)C=1C(CCC1)=O.C(C(C)(C)C)(=O)O.CC(C([O-])([O-])[O-])(C)C>>O=C1C(C(CC1)CC(=O)OC)=CCCCC
C[C:12](C)(C)[C:13](=[O:14])[OH:15].CC(C)(C([O-])([O-])[O-])[CH3:16].O[CH:5]([CH2:4][CH2:3][CH2:2][CH3:1])[C:6]1=[CH:11][CH2:10][CH2:9][C:7]1=[O:8]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]=[C:6]1[C:7](=[O:8])[CH2:9][CH2:10][CH:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]
CC(C)(C)C(=O)O.CC(C)(C)C([O-])([O-])[O-].CCCCC(O)C1=CCCC1=O
CCCCC=C1C(=O)CCC1CC(=O)OC
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
5a427e86cb728b62e97e3a9b8761cbd0f04cf303e69df89d58c25172edfe9b0c
bc537d2de7ba3dc6bb8984e8defe531f2d8495eed6447f40b3da4cb7e1cd3a44
[CH]=C1CCCC1=O
C-C(-C)(-[CH3;D1;+0:1])-C(-[O-])(-[O-])-[O-].C-[C;H0;D4;+0:2](-C)(-C)-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5].O-[CH;D3;+0:6](-[C:7]-[C:8])-[C;H0;D3;+0:9]1=[CH;D2;+0:10]-[C:11]-[C:12]-[C:13]-1=[O;D1;H0:14]>>[C:8]-[C:7]-[CH;D2;+0:6]=[C;H0;D3;+0:9]1-[C:13](=[O;D1;H0:14])-[C:12]-[C:11]-[CH;D3;+0:10]-1-[CH2;D2;+0:2]-[C:3](=[O;D1;H...
88
[{"value": 88.0, "product": "O=C1C(C(CC1)CC(=O)OC)=CCCCC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 2-(1-hydroxypentyl)-2-cyclopenten-1-one (720 mg, 4.2 mmol) and pivalic acid (100 mg, 0.98 mmol) in trimethylorthoacetate (5 ml, 39.3 mmol) was heated at 115° C. for 3 hours with distillation of MeOH. The concentrated reaction mixture was bulb-to-bulb distilled to afford the title compound in 88% yield and ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ketone.Secondary alcohol
Ketone.Ester
C1=CCCC1
C1CCCC1
C1CCCC1
HO-
CO
null
null
CC(C)(C)C(=O)O.CC(C)(C)C([O-])([O-])[O-].CCCCC(O)C1=CCCC1=O>CO>CCCCC=C1C(=O)CCC1CC(=O)OC
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2bb76cb3b2ce428c869ec19cde483fb2
O=C(F)C(F)(C(F)(F)F)C(F)(F)F.OCCCOCCCO>>O=C(OCCCOCCCOC(=O)C(F)(C(F)(F)F)C(F)(F)F)C(F)(C(F)(F)F)C(F)(F)F
OCCCOCCCO.FC(=O)C(F)(C(F)(F)F)C(F)(F)F>>C(F)(C(F)(F)F)(C(F)(F)F)C(=O)OCCCOCCCOC(=O)C(F)(C(F)(F)F)C(F)(F)F
[C:12](=[O:13])([C:14]([F:15])([C:16]([F:17])([F:19])[F:23])[C:30]([F:31])([F:32])[F:33])[F:25].[OH:1][CH2:2][CH2:9][CH2:8][O:7][CH2:6][CH2:5][CH2:4][OH:3]>>[O:1]=[C:2]([O:3][CH2:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][CH2:10][O:11][C:12](=[O:13])[C:14]([F:15])([C:16]([F:17])([F:18])[F:19])[C:20]([F:21])([F:22])[F:23])[C:2...
O=C(F)C(F)(C(F)(F)F)C(F)(F)F.OCCCOCCCO
O=C(OCCCOCCCOC(=O)C(F)(C(F)(F)F)C(F)(F)F)C(F)(C(F)(F)F)C(F)(F)F
null
null
null
Acylation
OtherReaction
e4d30fe38ff87c2481c7f22c259cbc2c34987aa16c61c63d81a7a542c909ff2e
599255592d198b68bb8a6598b0274efd9cfd7815bf5288af70012aec84cc494d
null
[#8:1]-[C:2]-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[OH;D1;+0:5].[C:6]-[C:7]-[OH;D1;+0:8].[F;D1;H0:9]-[C;H0;D4;+0:10](-[C;H0;D3;+0:11](-[F;H0;D1;+0:12])=[O;D1;H0:13])(-[C;H0;D4;+0:14](-[F;D1;H0:15])(-[F;D1;H0:16])-[F;H0;D1;+0:17])-[C;H0;D4;+0:18](-[F;D1;H0:19])(-[F;D1;H0:20])-[F;D1;H0:21]>>[#8:1]-[C:2]-[CH2;D2;+0:3]-[C:22]-[#8:23...
92.1
[{"value": 81.0, "product": "C(F)(C(F)(F)F)(C(F)(F)F)C(=O)OCCCOCCCOC(=O)C(F)(C(F)(F)F)C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.1, "product": "C(F)(C(F)(F)F)(C(F)(F)F)C(=O)OCCCOCCCOC(=O)C(F)(C(F)(F)F)C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
7
HOUR
HO(CH2)3O(CH2)3OH (10 g) was loaded into an autoclave and stirred in a sealed state, and FCOCF(CF3)2 (36.95 g) was fed over 7 hours at room temperature with occasional pauses for bubbling with nitrogen gas under unsealed conditions. After the feeding, the reaction solution was stirred at room temperature for 1 hour and...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Trifluoro group.Trifluoro group.Tertiary halide.Primary alcohol.Primary alcohol
Trifluoro group.Trifluoro group.Trifluoro group.Trifluoro group.Tertiary halide.Tertiary halide.Ester.Ester
null
null
null
Other
null
null
7
O=C(F)C(F)(C(F)(F)F)C(F)(F)F.OCCCOCCCO>>O=C(OCCCOCCCOC(=O)C(F)(C(F)(F)F)C(F)(F)F)C(F)(C(F)(F)F)C(F)(F)F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-bb577df9e2c347328109835fd6a602b1
Cc1ccc(S(=O)(=O)OC(C)COC(C)(C)C)cc1.OCCCO>>CC(COC(C)(C)C)OCCCO
Cl.[OH-].[K+].OCCCO.S(=O)(=O)(C1=CC=C(C)C=C1)OC(C)COC(C)(C)C>>OCCCOC(C)COC(C)(C)C
Cc1ccc(S(=O)(=O)O[CH:2]([CH3:1])[CH2:3][O:4][C:5]([CH3:6])([CH3:7])[CH3:8])cc1.[OH:9][CH2:10][CH2:11][CH2:12][OH:13]>>[CH3:1][CH:2]([CH2:3][O:4][C:5]([CH3:6])([CH3:7])[CH3:8])[O:9][CH2:10][CH2:11][CH2:12][OH:13]
Cc1ccc(S(=O)(=O)OC(C)COC(C)(C)C)cc1.OCCCO
CC(COC(C)(C)C)OCCCO
null
null
O1CCOCC1
Heteroatom Alkylation and Arylation
OtherReaction
14f213034e6a37dd0cb837e56b2a221a4a43776111e112dda97ccbb323c0e76d
603fcf095026d2fb605fcefe86430c369a5441c61b94694e2075fffc1fd129c3
null
C-c1:c:c:c(-S(=O)(=O)-O-[CH;D3;+0:1](-[C;D1;H3:2])-[C:3]-[#8:4]-[C:5](-[C;D1;H3:6])(-[C;D1;H3:7])-[C;D1;H3:8]):c:c:1.[C:9]-[C:10]-[OH;D1;+0:11]>>[C:9]-[C:10]-[O;H0;D2;+0:11]-[CH;D3;+0:1](-[C;D1;H3:2])-[C:3]-[#8:4]-[C:5](-[C;D1;H3:6])(-[C;D1;H3:7])-[C;D1;H3:8]
43.8
[{"value": 43.8, "product": "OCCCOC(C)COC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Potassium hydroxide (274.27 g) and HO(CH2)3OH (371.93 g) were added to dioxane (3 L), and then TsOCH(CH3)CH2OC(CH3)3 (700 g) prepared in Example 2-1 was added gradually. The reaction solution was refluxed with heating for 16 hours, allowed to cool, and poured onto ice (500 g), neutralized with 2 N hydrochloric acid, co...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Primary alcohol
Ether
c1ccccc1
null
null
TsOH.HO-
O1CCOCC1
null
null
Cc1ccc(S(=O)(=O)OC(C)COC(C)(C)C)cc1.OCCCO>O1CCOCC1>CC(COC(C)(C)C)OCCCO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-86d261b188c3472ea1e89fc68be3f816
CC(COC(C)(C)C)OCCCO>>CC(CO)OCCCO
OCCCOC(C)COC(C)(C)C.Cl>>OCCCOC(C)CO
CC(C)(C)[O:4][CH2:3][CH:2]([CH3:1])[O:5][CH2:6][CH2:7][CH2:8][OH:9]>>[CH3:1][CH:2]([CH2:3][OH:4])[O:5][CH2:6][CH2:7][CH2:8][OH:9]
CC(COC(C)(C)C)OCCCO
CC(CO)OCCCO
null
null
null
Deprotection
Ether cleavage to primary alcohol
9614211a2a35d6177bcded67d8911ba46072c6f11693f23436d14d3c121d33af
29a81fd08d26edc3da6d72c4958026f5af2119326dc1b4714ee5be1c41835609
null
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[OH;D1;+0:1]
91.3
[{"value": 91.3, "product": "OCCCOC(C)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
HO(CH2)3OCH(CH3)CH2OC(CH3)3 (203.39 g) prepared in Example 2-2 was loaded into a round-bottomed flask and stirred with 5 N hydrochloric acid (1 L) at room temperature for 43 hours. The reaction solution was concentrated with an evaporator, and then, after addition of toluene, concentrated again with an evaporator to gi...
10.6084/m9.figshare.5104873.v1
null
Ether
Primary alcohol
null
null
null
Other
null
null
null
CC(COC(C)(C)C)OCCCO>>CC(CO)OCCCO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c4229ab0dce14b9886f55da78a21d461
CC(CO)OCCCO.O=C(F)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F>>CC(COC(=O)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F)OCCCOC(=O)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F
C(F)(F)(F)C(F)(F)C(F)(F)OC(F)(C(F)(F)F)C(F)(F)OC(F)(C(F)(F)F)C(=O)F.OCCCOC(C)CO>>C(F)(F)(F)C(F)(F)C(F)(F)OC(F)(C(F)(F)F)C(F)(F)OC(F)(C(F)(F)F)C(=O)OCC(C)OCCCOC(=O)C(F)(C(F)(F)F)OC(F)(F)C(F)(C(F)(F)F)OC(F)(F)C(F)(F)C(F)(F)F
[CH3:1][CH:2]([CH2:3][OH:4])[O:34][CH2:35][CH2:36][CH2:37][OH:38].[C:5](=[O:6])([C:7]([F:8])([O:9][C:10]([F:11])([F:12])[C:13]([F:14])([O:15][C:16]([F:17])([F:18])[C:19]([F:20])([C:22]([F:23])([F:25])[F:59])[F:51])[C:26]([F:27])([F:28])[F:29])[C:30]([F:21])([F:48])[F:67])[F:42]>>[CH3:1][CH:2]([CH2:3][O:4][C:5](=[O:6])[...
CC(CO)OCCCO.O=C(F)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F
CC(COC(=O)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F)OCCCOC(=O)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F
null
null
C(=O)(O)[O-].[Na+]
Acylation
OtherReaction
ecf64c3d7829aa41163740b7b8b48d17ced9b305fb54f4144a94331afc334222
b5800ccc1456e0f7e50a5b399bc5dd10000c4999d7d141f4411fd3d30d4028f2
null
[#8:1]-[C:2](-[F;D1;H0:3])(-[C;H0;D3;+0:4](-[F;H0;D1;+0:5])=[O;D1;H0:6])-[C;H0;D4;+0:7](-[F;H0;D1;+0:8])(-[F;H0;D1;+0:9])-[F;H0;D1;+0:10].[#8:11]-[C:12](-[F;D1;H0:13])(-[F;D1;H0:14])-[C;H0;D4;+0:15](-[F;D1;H0:16])(-[F;H0;D1;+0:17])-[C;H0;D4;+0:18](-[F;D1;H0:19])(-[F;D1;H0:20])-[F;H0;D1;+0:21].[C:22]-[C:23]-[OH;D1;+0:24...
null
[]
null
null
2
HOUR
CF3(CF2)2OCF(CF3)CF2OCF(CF3)COF (120.69 g) was loaded into an autoclave and stirred under a nitrogen stream, and HO(CH2)3OCH(CH3)CH2OH (15.1 g) prepared in Example 2-3 was fed over 2 hours, while the temperature in the autoclave was maintained at 30° C. or below. Then, the reaction solution was stirred at room temperat...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Trifluoro group.Trifluoro group.Tertiary halide.Tertiary halide.Primary alcohol.Primary alcohol
Trifluoro group.Trifluoro group.Trifluoro group.Trifluoro group.Trifluoro group.Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Ester.Ester.Ether.Ether
null
null
null
Other
C(=O)(O)[O-].[Na+]
null
2
CC(CO)OCCCO.O=C(F)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F>C(=O)(O)[O-].[Na+]>CC(COC(=O)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F)OCCCOC(=O)C(F)(OC(F)(F)C(F)(OC(F)(F)C(F)(F)C(F)(F)F)C(F)(F)F)C(F)(F)F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9b383dcedcb34a41bc0685aba01455b8
Cc1cc(C(C)(C)C)cc(C)c1S(=O)(=O)Cl.Cc1cc(C(C)(C)C)cc(C)c1S(=O)(=O)Cl>>Cc1cc(C(C)(C)C)cc(C)c1SSc1c(C)cc(C(C)(C)C)cc1C
CC1=C(C(=CC(=C1)C(C)(C)C)C)S(=O)(=O)Cl.CC1=C(C(=CC(=C1)C(C)(C)C)C)S(=O)(=O)Cl>>CC1=C(C(=CC(=C1)C(C)(C)C)C)SSC1=C(C=C(C=C1C)C(C)(C)C)C
O=[S:13](=O)(Cl)[c:12]1[c:2]([CH3:1])[cH:3][c:4]([C:5]([CH3:6])([CH3:7])[CH3:8])[cH:9][c:10]1[CH3:11].O=[S:14](=O)(Cl)[c:15]1[c:16]([CH3:17])[cH:18][c:19]([C:20]([CH3:21])([CH3:22])[CH3:23])[cH:24][c:25]1[CH3:26]>>[CH3:1][c:2]1[cH:3][c:4]([C:5]([CH3:6])([CH3:7])[CH3:8])[cH:9][c:10]([CH3:11])[c:12]1[S:13][S:14][c:15]1[c...
Cc1cc(C(C)(C)C)cc(C)c1S(=O)(=O)Cl.Cc1cc(C(C)(C)C)cc(C)c1S(=O)(=O)Cl
Cc1cc(C(C)(C)C)cc(C)c1SSc1c(C)cc(C(C)(C)C)cc1C
null
[Ti](Cl)(Cl)(Cl)Cl.[Zn].[Ti](Cl)(Cl)(Cl)Cl
O1CCCC1
Miscellaneous
OtherReaction
89bc08fe361ff61a489f484f20679a7df55a48107f2c39ffd1d09581fd50c810
9c42b3da034c86ee612727af954fc5bd394c43d40a029338ed887589dff65e6a
c1ccc(SSc2ccccc2)cc1
Cl-[S;H0;D4;+0:1](=O)(=O)-[c:2](:[c:3]):[c:4].Cl-[S;H0;D4;+0:5](=O)(=O)-[c:6](:[c:7]):[c:8]>>[c:3]:[c:2](-[S;H0;D2;+0:1]-[S;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]):[c:4]
64.1
[{"value": 64.1, "product": "CC1=C(C(=CC(=C1)C(C)(C)C)C)SSC1=C(C=C(C=C1C)C(C)(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
null
null
A two liter, three-neck flask, was obtained. A condenser with a drying tube, a thermometer, and a dropping funnel were each attached to the flask. Zinc dust (<10 micron, 43.6 g, 0.667 mol) and anhydrous tetrahydrofuran (400 mL) were added to the flask. The mixture was stirred and cooled on an ice-water bath and 58.6 ml...
10.6084/m9.figshare.5104873.v1
null
Sulfonyl halide.Sulfonyl halide
Disulfide
null
null
c1ccccc1.c1ccccc1
Other
[Ti](Cl)(Cl)(Cl)Cl.[Zn].[Ti](Cl)(Cl)(Cl)Cl.O1CCCC1
60
null
Cc1cc(C(C)(C)C)cc(C)c1S(=O)(=O)Cl.Cc1cc(C(C)(C)C)cc(C)c1S(=O)(=O)Cl>[Ti](Cl)(Cl)(Cl)Cl.[Zn].[Ti](Cl)(Cl)(Cl)Cl.O1CCCC1>Cc1cc(C(C)(C)C)cc(C)c1SSc1c(C)cc(C(C)(C)C)cc1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-168c4fd7432548b4be25c5e932775b2c
FC(c1ccccc1)C(F)c1ccccc1>>FC(F)C(c1ccccc1)c1ccccc1
FC(C(C1=CC=CC=C1)F)C1=CC=CC=C1.CC1=C(C(=CC(=C1)C(C)(C)C)C)S(F)(F)F.C1=CC=C(C=C1)[C@H]([C@H](C2=CC=CC=C2)O)O>>FC(C(C1=CC=CC=C1)C1=CC=CC=C1)F
[F:1][CH:2]([CH:4]([F:3])[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1>>[F:1][CH:2]([F:3])[CH:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
FC(c1ccccc1)C(F)c1ccccc1
FC(F)C(c1ccccc1)c1ccccc1
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
33f5eee389135328e4ea80739281a0fec05a7ae4bbeb419b986075f2c964da81
715caf9c0ed0a006b1bedb353e5a492fd2cef4b9382daa4b0a254715d87abe0a
c1ccc(Cc2ccccc2)cc1
[F;D1;H0:1]-[CH;D3;+0:2](-[CH;D3;+0:3](-[F;H0;D1;+0:4])-[c:5](:[c:6]):[c:7])-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]>>[F;D1;H0:1]-[CH;D3;+0:2](-[F;H0;D1;+0:4])-[CH;D3;+0:3](-[c:5](:[c:6]):[c:7])-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]
0.03
[{"value": 0.03, "product": "FC(C(C1=CC=CC=C1)C1=CC=CC=C1)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
In a 15 mL fluoropolymer flask, 2,6-dimethyl-4-tert-butylphenylsulfur trifluoride (0.625 g, 2.5 mmol) was dissolved in 5 mL of anhydrous CH2Cl2. A solution of meso-1,2-diphenyl-1,2-ethanediol (0.214 g, 1.0 mmol) in 5 mL of anhydrous CH2Cl2 was added to the above stirred solution at room temperature. After 3 hours, C12H...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Secondary halide
Secondary halide.Secondary halide
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
null
C(Cl)Cl
null
3
FC(c1ccccc1)C(F)c1ccccc1>C(Cl)Cl>FC(F)C(c1ccccc1)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-da4e90e4acbe4d3ca8e30de0142f42ff
O=C(Cl)c1ccccc1.O=C(Nc1ccn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2O)c(=O)n1)c1ccccc1>>O=C(Nc1ccn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2OC(=O)c2ccccc2)c(=O)n1)c1ccccc1
C(C1=CC=CC=C1)(=O)NC1=NC(N(C=C1)[C@H]1[C@H](O)[C@H](O)[C@H](O)CO1)=O.C(=O)(C1=CC=CC=C1)Cl.C(CC)O>>C(C1=CC=CC=C1)(=O)NC1=NC(N(C=C1)[C@H]1[C@H](OC(C2=CC=CC=C2)=O)[C@H](O)[C@H](O)CO1)=O
Cl[C:17](=[O:18])[c:19]1[cH:20][cH:21][cH:22][cH:23][cH:24]1.[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][n:7]([C@@H:8]2[O:9][CH2:10][C@@H:11]([OH:12])[C@@H:13]([OH:14])[C@H:15]2[OH:16])[c:25](=[O:26])[n:27]1)[c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][n:7]([C@@H:8]2[O:9][CH2:10][C@@H:11](...
O=C(Cl)c1ccccc1.O=C(Nc1ccn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2O)c(=O)n1)c1ccccc1
O=C(Nc1ccn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2OC(=O)c2ccccc2)c(=O)n1)c1ccccc1
null
null
N1=CC=CC=C1.CN(C=O)C
Acylation
Schotten-Baumann to ester
27b76e29491fa7db5375755e15223de884a194f57a493147db0b5495ea981908
d47ab90ace9b5dcd818151c10aae400dcf599f5a3476072b8dfedc474e97c335
O=C(Nc1ccn([C@@H]2OCCC[C@H]2OC(=O)c2ccccc2)c(=O)n1)c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[#8:6]-[C:7]-[C:8](-[OH;D1;+0:9])-[C:10]>>[#8:6]-[C:7]-[C:8](-[O;H0;D2;+0:9]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5])-[C:10]
null
[]
124
CELSIUS
8
HOUR
54.0 g (0.155 mol) of N4-benzoyl-1-(β-D-ribopyranosyl)cytosine 1 were dissolved in 830 ml of dimethylformamide (DMF) and 1.5 l of pyridine (both solvents dried and stored over molecular sieve 3 Å) with warming to 124° C. 23.0 g (0.163 mol; 1.05 eq.) of BzCl, dissolved in 210 ml of pyridine, were added dropwise at −58° ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary alcohol
Ester
null
null
c1cncnc1.C1CCOCC1.c1ccccc1.c1ccccc1
HCl
N1=CC=CC=C1.CN(C=O)C
124
8
O=C(Cl)c1ccccc1.O=C(Nc1ccn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2O)c(=O)n1)c1ccccc1>N1=CC=CC=C1.CN(C=O)C>O=C(Nc1ccn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2OC(=O)c2ccccc2)c(=O)n1)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-97d2f9493a204b48a562afb3c9143e01
O=C(Cl)c1ccccc1.O=C(c1ccccc1)N(C(=O)c1ccccc1)c1ncnc2c1ncn2[C@@H]1OC[C@@H](O)[C@@H](O)[C@H]1O>>O=C(O[C@@H]1[C@H](O)[C@H](O)CO[C@H]1n1cnc2c(N(C(=O)c3ccccc3)C(=O)c3ccccc3)ncnc21)c1ccccc1
C(C1=CC=CC=C1)(=O)N(C1=C2N=CN(C2=NC=N1)[C@H]1[C@H](O)[C@H](O)[C@H](O)CO1)C(C1=CC=CC=C1)=O.C(=O)(C1=CC=CC=C1)Cl>>C(C1=CC=CC=C1)(=O)N(C1=C2N=CN(C2=NC=N1)[C@H]1[C@H](OC(C2=CC=CC=C2)=O)[C@H](O)[C@H](O)CO1)C(C1=CC=CC=C1)=O
Cl[C:2](=[O:1])[c:38]1[cH:39][cH:40][cH:41][cH:42][cH:43]1.[OH:3][C@@H:4]1[C@H:5]([OH:6])[C@H:7]([OH:8])[CH2:9][O:10][C@H:11]1[n:12]1[cH:13][n:14][c:15]2[c:16]([N:17]([C:18](=[O:19])[c:20]3[cH:21][cH:22][cH:23][cH:24][cH:25]3)[C:26](=[O:27])[c:28]3[cH:29][cH:30][cH:31][cH:32][cH:33]3)[n:34][cH:35][n:36][c:37]12>>[O:1]=...
O=C(Cl)c1ccccc1.O=C(c1ccccc1)N(C(=O)c1ccccc1)c1ncnc2c1ncn2[C@@H]1OC[C@@H](O)[C@@H](O)[C@H]1O
O=C(O[C@@H]1[C@H](O)[C@H](O)CO[C@H]1n1cnc2c(N(C(=O)c3ccccc3)C(=O)c3ccccc3)ncnc21)c1ccccc1
null
CN(C)C=1C=CN=CC1
N1=CC=CC=C1.C(Cl)Cl
Acylation
Schotten-Baumann to ester
27b76e29491fa7db5375755e15223de884a194f57a493147db0b5495ea981908
d47ab90ace9b5dcd818151c10aae400dcf599f5a3476072b8dfedc474e97c335
O=C(O[C@@H]1CCCO[C@H]1n1cnc2c(N(C(=O)c3ccccc3)C(=O)c3ccccc3)ncnc21)c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[#8:6]-[C:7]-[C:8](-[OH;D1;+0:9])-[C:10]>>[#8:6]-[C:7]-[C:8](-[O;H0;D2;+0:9]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5])-[C:10]
72.1
[{"value": 72.1, "product": "C(C1=CC=CC=C1)(=O)N(C1=C2N=CN(C2=NC=N1)[C@H]1[C@H](OC(C2=CC=CC=C2)=O)[C@H](O)[C@H](O)CO1)C(C1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-88.5
CELSIUS
60
HOUR
26.4 g (55,5 mmol) of 3 were dissolved in 550 ml of anhydrous CH2Cl2 and 55 ml of pyridine (in each case stored over a molecular sieve) under an N2 atmosphere, treated with 0.73 g (5.55 mmol; 0.1 eq.) of DMAP and cooled to −87 to −90° C. 8.58 g (61 mmol; 1.1 eq.) of BzCl in 14 ml of pyridine were added dropwise in the ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary alcohol
Ester
null
null
C1CCOCC1.c1ccccc1.c1ccccc1.c1ncnc2[nH]cnc12.c1ccccc1
HCl
CN(C)C=1C=CN=CC1.N1=CC=CC=C1.C(Cl)Cl
-88.5
60
O=C(Cl)c1ccccc1.O=C(c1ccccc1)N(C(=O)c1ccccc1)c1ncnc2c1ncn2[C@@H]1OC[C@@H](O)[C@@H](O)[C@H]1O>CN(C)C=1C=CN=CC1.N1=CC=CC=C1.C(Cl)Cl>O=C(O[C@@H]1[C@H](O)[C@H](O)CO[C@H]1n1cnc2c(N(C(=O)c3ccccc3)C(=O)c3ccccc3)ncnc21)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-74d1b8c5c2d54549b4a2b033dc7f78d5
O=C(Cl)c1ccccc1.O=C1c2ccccc2C(=O)N1CCc1cn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2O)c(=O)[nH]c1=O>>O=C(O[C@@H]1[C@H](O)[C@H](O)CO[C@H]1n1cc(CCN2C(=O)c3ccccc3C2=O)c(=O)[nH]c1=O)c1ccccc1
[Cl-].[NH4+].C1(C=2C(C(N1CCC=1C(NC(N(C1)[C@H]1[C@H](O)[C@H](O)[C@H](O)CO1)=O)=O)=O)=CC=CC2)=O.C(C1=CC=CC=C1)(=O)Cl>>C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](OC[C@H]([C@H]1O)O)N1C(=O)NC(=O)C(=C1)CCN1C(C=2C(C1=O)=CC=CC2)=O
Cl[C:2](=[O:1])[c:33]1[cH:34][cH:35][cH:36][cH:37][cH:38]1.[OH:3][C@@H:4]1[C@H:5]([OH:6])[C@H:7]([OH:8])[CH2:9][O:10][C@H:11]1[n:12]1[cH:13][c:14]([CH2:15][CH2:16][N:17]2[C:18](=[O:19])[c:20]3[cH:21][cH:22][cH:23][cH:24][c:25]3[C:26]2=[O:27])[c:28](=[O:29])[nH:30][c:31]1=[O:32]>>[O:1]=[C:2]([O:3][C@@H:4]1[C@H:5]([OH:6]...
O=C(Cl)c1ccccc1.O=C1c2ccccc2C(=O)N1CCc1cn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2O)c(=O)[nH]c1=O
O=C(O[C@@H]1[C@H](O)[C@H](O)CO[C@H]1n1cc(CCN2C(=O)c3ccccc3C2=O)c(=O)[nH]c1=O)c1ccccc1
null
null
N1=CC=CC=C1.ClCCl
Acylation
Schotten-Baumann to ester
27b76e29491fa7db5375755e15223de884a194f57a493147db0b5495ea981908
d47ab90ace9b5dcd818151c10aae400dcf599f5a3476072b8dfedc474e97c335
O=C(O[C@@H]1CCCO[C@H]1n1cc(CCN2C(=O)c3ccccc3C2=O)c(=O)[nH]c1=O)c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[#8:6]-[C:7]-[C:8](-[OH;D1;+0:9])-[C:10]>>[#8:6]-[C:7]-[C:8](-[O;H0;D2;+0:9]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5])-[C:10]
60,597.3
[{"value": 60.0, "product": "C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](OC[C@H]([C@H]1O)O)N1C(=O)NC(=O)C(=C1)CCN1C(C=2C(C1=O)=CC=CC2)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 60597.3, "product": "C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](OC[C@H]([C@H]1O)O)N1C(=O)NC(=O)C(=C1)CCN1C(C=2C(C1=O)=CC=CC2)=O", "details": "CAL...
-70
CELSIUS
35
MINUTE
10.6 g (0.025 mmol) of 5-(2-phtalimidoethyl)-1-(β-D-ribopyranosyl)uracil were dissolved in 20 ml of pyridine in a heated and argon-flushed 1 l four-necked flask and mixed with 200 ml of dichloromethane. The mixture was cooled to −70° C., 3.82 ml (0.033 mmol) of benzoyl chloride in 5 ml of pyridine and 20 ml of dichloro...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary alcohol
Ester
null
null
C1CCOCC1.c1cncnc1.c1ccc2c(c1)C[NH]C2.c1ccccc1
HCl
N1=CC=CC=C1.ClCCl
-70
0.583333
O=C(Cl)c1ccccc1.O=C1c2ccccc2C(=O)N1CCc1cn([C@@H]2OC[C@@H](O)[C@@H](O)[C@H]2O)c(=O)[nH]c1=O>N1=CC=CC=C1.ClCCl>O=C(O[C@@H]1[C@H](O)[C@H](O)CO[C@H]1n1cc(CCN2C(=O)c3ccccc3C2=O)c(=O)[nH]c1=O)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8e68a2667e8044979cef6c0524dbcd71
COc1ccc(NC(=O)Cc2ccc(C(F)(F)F)cc2)cc1OC>>COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC
COC=1C=C(C=CC1OC)NC(CC1=CC=C(C=C1)C(F)(F)F)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3].O.Cl>>COC=1C=C(C=CC1OC)NCCC1=CC=C(C=C1)C(F)(F)F
O=[C:8]([NH:7][c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[c:21]([O:22][CH3:23])[cH:20]1)[CH2:9][c:10]1[cH:11][cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][cH:19]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([NH:7][CH2:8][CH2:9][c:10]2[cH:11][cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][cH:19]2)[cH:20][c:21]1[O:22][CH3:23]
COc1ccc(NC(=O)Cc2ccc(C(F)(F)F)cc2)cc1OC
COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC
null
null
C1CCOC1
Reduction
Reduction of secondary amides to amines
85b757f1833edc9e5c6365ee6b904683f414e7b9a5f9bfcfd7addca401447058
ab40188eef2f825df7003af0ffae31d0ce53d126542122535627d3d354cbc9fe
c1ccc(CCNc2ccccc2)cc1
O=[C;H0;D3;+0:1](-[#7:2]-[c:3])-[C:4]-[c:5]>>[c:5]-[C:4]-[CH2;D2;+0:1]-[#7:2]-[c:3]
24.5
[{"value": 24.0, "product": "COC=1C=C(C=CC1OC)NCCC1=CC=C(C=C1)C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 24.5, "product": "COC=1C=C(C=CC1OC)NCCC1=CC=C(C=C1)C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A mixture of 3 g (8.8 mmol) N-(3,4-Dimethoxy-phenyl)-2-(4-trifluoromethyl-phenyl)-acetamide and 1 g (26.3 mmol) LiAlH4 in 100 mL THF was stirred for 1 h at room temperature. Water and HCl aq. was added and the mixture was extracted with ethyl acetate. The combined organic phases were washed with water, dried with MgSO4...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
null
null
null
c1ccccc1.c1ccccc1
Other
C1CCOC1
null
1
COc1ccc(NC(=O)Cc2ccc(C(F)(F)F)cc2)cc1OC>C1CCOC1>COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b788071888c243319146f7e8d516f378
COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC.O=C(O)C(C(=O)OCc1ccccc1)c1ccccc1>>COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)OCc2ccccc2)c2ccccc2)cc1OC
COC=1C=C(C=CC1OC)NCCC1=CC=C(C=C1)C(F)(F)F.C(C1=CC=CC=C1)OC(C(C(=O)O)C1=CC=CC=C1)=O.CN(C)C(=[N+](C)C)ON1C2=C(C=CC=C2)N=N1.[B-](F)(F)(F)F.CCN(CC)CC>>C(C1=CC=CC=C1)OC(C(C(=O)N(CCC1=CC=C(C=C1)C(F)(F)F)C1=CC(=C(C=C1)OC)OC)C1=CC=CC=C1)=O
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([NH:7][CH2:8][CH2:9][c:10]2[cH:11][cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][cH:19]2)[cH:39][c:40]1[O:41][CH3:42].O[C:20](=[O:21])[CH:22]([C:23](=[O:24])[O:25][CH2:26][c:27]1[cH:28][cH:29][cH:30][cH:31][cH:32]1)[c:33]1[cH:34][cH:35][cH:36][cH:37][cH:38]1>>[CH3:1][O:2][c:3]1[c...
COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC.O=C(O)C(C(=O)OCc1ccccc1)c1ccccc1
COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)OCc2ccccc2)c2ccccc2)cc1OC
null
null
CN(C)C=O
Acylation
Acylation of Nitrogen Nucleophiles by Carboxylic Acids
ac72df6259d5d7baee7abdbd4706ef4b4627f86ead9dc94f0cefcfcb37c21def
c5e4172490b2731ba9322b68af56376edadc31ce0bb9a3dfdea23a1817a852fd
O=C(OCc1ccccc1)C(C(=O)N(CCc1ccccc1)c1ccccc1)c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[c:4])-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8].[C:9]-[C:10]-[NH;D2;+0:11]-[c:12](:[c:13]):[c:14]>>[C:8]-[#8:7]-[C:5](=[O;D1;H0:6])-[C:3](-[c:4])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:11](-[C:10]-[C:9])-[c:12](:[c:13]):[c:14]
29
[{"value": 29.0, "product": "C(C1=CC=CC=C1)OC(C(C(=O)N(CCC1=CC=C(C=C1)C(F)(F)F)C1=CC(=C(C=C1)OC)OC)C1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 28.9, "product": "C(C1=CC=CC=C1)OC(C(C(=O)N(CCC1=CC=C(C=C1)C(F)(F)F)C1=CC(=C(C=C1)OC)OC)C1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is...
null
null
16
HOUR
A mixture of 0.7 g (2.1 mmol) (3,4-Dimethoxy-phenyl)-[2-(4-trifluoromethyl-phenyl)-ethyl]-amine, 0.58 g (2.1 mmol) 2-phenyl-malonic acid monobenzylester (commercially available), 0.83 g (2.5 mmol) TBTU and 0.43 g (4.3 mmol) NEt3 in 15 mL DMF was stirred at room temperature for 16 h. After evaporation to dryness the res...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Tertiary amide
null
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
CN(C)C=O
null
16
COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC.O=C(O)C(C(=O)OCc1ccccc1)c1ccccc1>CN(C)C=O>COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)OCc2ccccc2)c2ccccc2)cc1OC
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-42b4a92494f34c55aa383bde8206dcfe
COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)OCc2ccccc2)c2ccccc2)cc1OC>>COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)O)c2ccccc2)cc1OC
C(C1=CC=CC=C1)OC(C(C(=O)N(CCC1=CC=C(C=C1)C(F)(F)F)C1=CC(=C(C=C1)OC)OC)C1=CC=CC=C1)=O>>COC=1C=C(C=CC1OC)N(C(C(C(=O)O)C1=CC=CC=C1)=O)CCC1=CC=C(C=C1)C(F)(F)F
c1ccc(C[O:25][C:23]([CH:22]([C:20]([N:7]([c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[c:33]([O:34][CH3:35])[cH:32]2)[CH2:8][CH2:9][c:10]2[cH:11][cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][cH:19]2)=[O:21])[c:26]2[cH:27][cH:28][cH:29][cH:30][cH:31]2)=[O:24])cc1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([N:7]([CH2:8][CH2:9][c:...
COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)OCc2ccccc2)c2ccccc2)cc1OC
COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)O)c2ccccc2)cc1OC
null
[Pd]
C(C)(=O)O.C(C)(=O)OCC
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C(Cc1ccccc1)N(CCc1ccccc1)c1ccccc1
[#7:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](=[O;D1;H0:6])-[O;H0;D2;+0:7]-C-c1:c:c:c:c:c:1>>[#7:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](=[O;D1;H0:6])-[OH;D1;+0:7]
null
[]
null
null
null
null
0.35 g (0.62 mmol) N-(3,4-Dimethoxy-phenyl)-2-phenyl-N-[2-(4-trifluoromethyl-phenyl)-ethyl]-malonamic acid benzyl ester in 20 mL ethyl acetate and 0.37 mL acetic acid was hydrogenated over Pd/C with atmospheric pressure of H2 for 16 h at room temperature. The catalyst was filtered off and the and the filtrate evaporate...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
c1ccccc1.c1ccccc1.c1ccccc1
Other
[Pd].C(C)(=O)O.C(C)(=O)OCC
null
null
COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)OCc2ccccc2)c2ccccc2)cc1OC>[Pd].C(C)(=O)O.C(C)(=O)OCC>COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)O)c2ccccc2)cc1OC
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-4b9d3f93ebc54ec0bf7376c8f134501f
CN.COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)O)c2ccccc2)cc1OC>>CNC(=O)C(C(=O)N(CCc1ccc(C(F)(F)F)cc1)c1ccc(OC)c(OC)c1)c1ccccc1
COC=1C=C(C=CC1OC)N(C(C(C(=O)O)C1=CC=CC=C1)=O)CCC1=CC=C(C=C1)C(F)(F)F.CN.CN(C)C(=[N+](C)C)ON1C2=C(C=CC=C2)N=N1.[B-](F)(F)(F)F.N1=CC=CC=C1>>COC=1C=C(C=CC1OC)N(C(C(C(=O)NC)C1=CC=CC=C1)=O)CCC1=CC=C(C=C1)C(F)(F)F
[CH3:1][NH2:2].O[C:3](=[O:4])[CH:5]([C:6](=[O:7])[N:8]([CH2:9][CH2:10][c:11]1[cH:12][cH:13][c:14]([C:15]([F:16])([F:17])[F:18])[cH:19][cH:20]1)[c:21]1[cH:22][cH:23][c:24]([O:25][CH3:26])[c:27]([O:28][CH3:29])[cH:30]1)[c:31]1[cH:32][cH:33][cH:34][cH:35][cH:36]1>>[CH3:1][NH:2][C:3](=[O:4])[CH:5]([C:6](=[O:7])[N:8]([CH2:9...
CN.COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)O)c2ccccc2)cc1OC
CNC(=O)C(C(=O)N(CCc1ccc(C(F)(F)F)cc1)c1ccc(OC)c(OC)c1)c1ccccc1
null
null
CN(C)C=O
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(Cc1ccccc1)N(CCc1ccccc1)c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[c:4])-[C:5](=[O;D1;H0:6])-[#7:7](-[C:8])-[c:9].[C;D1;H3:10]-[NH2;D1;+0:11]>>[C:8]-[#7:7](-[c:9])-[C:5](=[O;D1;H0:6])-[C:3](-[c:4])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:11]-[C;D1;H3:10]
16.3
[{"value": 16.0, "product": "COC=1C=C(C=CC1OC)N(C(C(C(=O)NC)C1=CC=CC=C1)=O)CCC1=CC=C(C=C1)C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 16.3, "product": "COC=1C=C(C=CC1OC)N(C(C(C(=O)NC)C1=CC=CC=C1)=O)CCC1=CC=C(C=C1)C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
A mixture of 16.2 mg (0.033 mmol) N-(3,4-Dimethoxy-phenyl)-2-phenyl-N-[2-(4-trifluoromethyl-phenyl)-ethyl]-malonamic acid, 15.5 mg (0.049 mmol) methylamine (commercially available), 13.8 mg (0.043 mmol) TBTU and 7.8 mg (0.09 mmol) pyridine in 2 mL DMF was shaken for 4 h at room temperature. The mixture was evaporated t...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HO-
CN(C)C=O
null
4
CN.COc1ccc(N(CCc2ccc(C(F)(F)F)cc2)C(=O)C(C(=O)O)c2ccccc2)cc1OC>CN(C)C=O>CNC(=O)C(C(=O)N(CCc1ccc(C(F)(F)F)cc1)c1ccc(OC)c(OC)c1)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-34500abe57a04c3db6dfd547c5979406
CN(C)C(=O)C(C(=O)O)c1ccccc1.COc1ccc(NCCc2ccc(OC)c(OC)c2)cc1>>COc1ccc(N(CCc2ccc(OC)c(OC)c2)C(=O)C(C(=O)N(C)C)c2ccccc2)cc1
COC=1C=C(C=CC1OC)CCNC1=CC=C(C=C1)OC.COC=1C=C(C=CC1OC)CCNC1=CC=C(C=C1)OC.CN(C(C(C(=O)O)C1=CC=CC=C1)=O)C.CN(C)C(=[N+](C)C)ON1C2=C(C=CC=C2)N=N1.[B-](F)(F)(F)F.CCN(C(C)C)C(C)C>>COC=1C=C(C=CC1OC)CCN(C(C(C(=O)N(C)C)C1=CC=CC=C1)=O)C1=CC=C(C=C1)OC
O[C:20](=[O:21])[CH:22]([C:23](=[O:24])[N:25]([CH3:26])[CH3:27])[c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1.[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([NH:7][CH2:8][CH2:9][c:10]2[cH:11][cH:12][c:13]([O:14][CH3:15])[c:16]([O:17][CH3:18])[cH:19]2)[cH:34][cH:35]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([N:7]([CH2:8][CH2:9][c:10]2[c...
CN(C)C(=O)C(C(=O)O)c1ccccc1.COc1ccc(NCCc2ccc(OC)c(OC)c2)cc1
COc1ccc(N(CCc2ccc(OC)c(OC)c2)C(=O)C(C(=O)N(C)C)c2ccccc2)cc1
null
null
CN(C)C=O
Acylation
Acylation of Nitrogen Nucleophiles by Carboxylic Acids
ac72df6259d5d7baee7abdbd4706ef4b4627f86ead9dc94f0cefcfcb37c21def
c5e4172490b2731ba9322b68af56376edadc31ce0bb9a3dfdea23a1817a852fd
O=C(Cc1ccccc1)N(CCc1ccccc1)c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[c:4])-[C:5](=[O;D1;H0:6])-[#7:7](-[C;D1;H3:8])-[C;D1;H3:9].[C:10]-[C:11]-[NH;D2;+0:12]-[c:13](:[c:14]):[c:15]>>[C:10]-[C:11]-[N;H0;D3;+0:12](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[c:4])-[C:5](=[O;D1;H0:6])-[#7:7](-[C;D1;H3:8])-[C;D1;H3:9])-[c:13](:[c:14]):[c:15]
61
[{"value": 61.0, "product": "COC=1C=C(C=CC1OC)CCN(C(C(C(=O)N(C)C)C1=CC=CC=C1)=O)C1=CC=C(C=C1)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 48.7, "product": "COC=1C=C(C=CC1OC)CCN(C(C(C(=O)N(C)C)C1=CC=CC=C1)=O)C1=CC=C(C=C1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
A mixture of 28.7 mg (0.1 mmol) [2-(3,4-Dimethoxy-phenyl)-ethyl]-(4-methoxy-phenyl)-amine (intermediate 2), 20.7 mg (0.1 mmol) N,N-Dimethyl-2-phenyl-malonamic acid (WO2000009481), 38.5 mg (0.12 mmol) TBTU and 38.7 mg (0.3 mmol) DIPEA in 3 mL DMF was stirred at room temperature for 16 h. The mixture was concentrated dil...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Tertiary amide
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HO-
CN(C)C=O
null
16
CN(C)C(=O)C(C(=O)O)c1ccccc1.COc1ccc(NCCc2ccc(OC)c(OC)c2)cc1>CN(C)C=O>COc1ccc(N(CCc2ccc(OC)c(OC)c2)C(=O)C(C(=O)N(C)C)c2ccccc2)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a175a90011cb4823bf69fdab4ee0fdf5
CCOC(=O)C(C)(C(=O)Cl)c1ccccc1.COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC>>CCOC(=O)C(C)(C(=O)N(CCc1ccc(C(F)(F)F)cc1)c1ccc(OC)c(OC)c1)c1ccccc1
COC=1C=C(C=CC1OC)NCCC1=CC=C(C=C1)C(F)(F)F.COC=1C=C(C=CC1OC)NCCC1=CC=C(C=C1)C(F)(F)F.C(C)OC(C(C)(C1=CC=CC=C1)C(=O)Cl)=O.C(C)N(CC)CC>>C(C)OC(C(C(=O)N(CCC1=CC=C(C=C1)C(F)(F)F)C1=CC(=C(C=C1)OC)OC)(C1=CC=CC=C1)C)=O
Cl[C:8]([C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[c:33]1[cH:34][cH:35][cH:36][cH:37][cH:38]1)=[O:9].[NH:10]([CH2:11][CH2:12][c:13]1[cH:14][cH:15][c:16]([C:17]([F:18])([F:19])[F:20])[cH:21][cH:22]1)[c:23]1[cH:24][cH:25][c:26]([O:27][CH3:28])[c:29]([O:30][CH3:31])[cH:32]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH...
CCOC(=O)C(C)(C(=O)Cl)c1ccccc1.COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC
CCOC(=O)C(C)(C(=O)N(CCc1ccc(C(F)(F)F)cc1)c1ccc(OC)c(OC)c1)c1ccccc1
null
null
null
Acylation
N-alkylation of secondary amines with alkyl halides
b92e0bfd3d683c1f2a209adfe70a67ad7cb0d87749eb59e8fe0cf1689bc291e0
96cb0a2fed10552c5770a45a2d6523b47ac3e38928b4a9c698d8577451182dcd
O=C(Cc1ccccc1)N(CCc1ccccc1)c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])(-[c:5])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9].[C:10]-[C:11]-[NH;D2;+0:12]-[c:13](:[c:14]):[c:15]>>[C:10]-[C:11]-[N;H0;D3;+0:12](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])(-[c:5])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9])-[c:13](:[c:14]):[c:15]
45
[{"value": 45.0, "product": "C(C)OC(C(C(=O)N(CCC1=CC=C(C=C1)C(F)(F)F)C1=CC(=C(C=C1)OC)OC)(C1=CC=CC=C1)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 45.0, "product": "C(C)OC(C(C(=O)N(CCC1=CC=C(C=C1)C(F)(F)F)C1=CC(=C(C=C1)OC)OC)(C1=CC=CC=C1)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": fal...
null
null
16
HOUR
A mixture of 97.5 mg (0.3 mmol) (3,4-dimethoxy-phenyl)-[2-(4-trifluoromethyl-phenyl)-ethyl]-amine (intermediate 1), 101 mg (0.45 mmol) 2-chlorocarbonyl-2-phenyl-propionic acid ethyl ester (Journal of Organic Chemistry (1959), 24 109-10) and 121 mg (1.2 mmol) triethylamine 15 mL DCM was stirred for 16 h at room temperat...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary amine
Tertiary amide
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HCl
null
null
16
CCOC(=O)C(C)(C(=O)Cl)c1ccccc1.COc1ccc(NCCc2ccc(C(F)(F)F)cc2)cc1OC>>CCOC(=O)C(C)(C(=O)N(CCc1ccc(C(F)(F)F)cc1)c1ccc(OC)c(OC)c1)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8a3c4571d07c44b796fe00511e454f86
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Cl)CCC1>>COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)CCC1
C(C)(C)N(CC)C(C)C.ClC1=CC(CCC1)=O.COCCOCC1=C(C(=O)O)C=CC(=N1)C(F)(F)F.C1(=CC=CC=C1)C.C1(=CC=CC=C1)C>>COCCOCC1=NC(=CC=C1C(=O)OC1=CC(CCC1)=O)C(F)(F)F
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][c:7]1[n:8][c:9]([C:10]([F:11])([F:12])[F:13])[cH:14][cH:15][c:16]1[C:17](=[O:18])[OH:19].Cl[C:20]1=[CH:21][C:22](=[O:23])[CH2:24][CH2:25][CH2:26]1>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][c:7]1[n:8][c:9]([C:10]([F:11])([F:12])[F:13])[cH:14][cH:15][c:16]1[C:17](=[O:18])[O:19][C:20]1...
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Cl)CCC1
COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)CCC1
null
[Cl-].[Cl-].[Zn+2]
ClCCl.O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
fcf8f2bb951391d4eca3e180ca1db9de221ab19064c43fbc3ee25d99eb3d4dbc
83fa46670fde4697f2da46ad00486528b93f00a3ef192db8e938bfe22fc495ff
O=C1C=C(OC(=O)c2cccnc2)CCC1
Cl-[C;H0;D3;+0:1]1=[C:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6]-[C:7]-1.[#7;a:8]:[c:9]:[c:10]-[C:11](=[O;D1;H0:12])-[OH;D1;+0:13]>>[#7;a:8]:[c:9]:[c:10]-[C:11](=[O;D1;H0:12])-[O;H0;D2;+0:13]-[C;H0;D3;+0:1]1=[C:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6]-[C:7]-1
null
[]
null
null
null
null
To a mixture of 157 mg (1.15 mmol) of 3-chlorocyclohex-2-en-1-one, 16 mg (0.12 mmol) of ZnCl2, 324 mg (1.15 mmol) of 2-methoxyethoxymethyl-6-trifluoromethylnicotinic acid (preparation described in WO 2001094339) and 2 ml of toluene there are added dropwise, under a nitrogen atmosphere, over the course of 15 minutes, 16...
10.6084/m9.figshare.5104873.v1
null
Alkenyl halide.Carboxylic acid
Ester
C1=CCCCC1
C1=CCCCC1
c1ccncc1.C1=CCCCC1
HCl
[Cl-].[Cl-].[Zn+2].ClCCl.O
null
null
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Cl)CCC1>[Cl-].[Cl-].[Zn+2].ClCCl.O>COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)CCC1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e08e1cbc6beb424492820e89b8e50368
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Cl)C2CCC1C2>>COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)C2CCC1C2
C1(=CC=CC=C1)C.ClC1=CC(C2CCC1C2)=O.COCCOCC1=C(C(=O)O)C=CC(=N1)C(F)(F)F.C(C)(C)N(CC)C(C)C>>COCCOCC1=NC(=CC=C1C(=O)OC1=CC(C2CCC1C2)=O)C(F)(F)F
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][c:7]1[n:8][c:9]([C:10]([F:11])([F:12])[F:13])[cH:14][cH:15][c:16]1[C:17](=[O:18])[OH:19].Cl[C:20]1=[CH:21][C:22](=[O:23])[CH:24]2[CH2:25][CH2:26][CH:27]1[CH2:28]2>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][c:7]1[n:8][c:9]([C:10]([F:11])([F:12])[F:13])[cH:14][cH:15][c:16]1[C:17](=[O:1...
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Cl)C2CCC1C2
COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)C2CCC1C2
null
[Cl-].[Cl-].[Zn+2]
ClCCl
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
b0cc2671c5188ff45d2dc8f6f4a2748058b058251e35db4909cb7151f9e28dbd
83fa46670fde4697f2da46ad00486528b93f00a3ef192db8e938bfe22fc495ff
O=C(OC1=CC(=O)C2CCC1C2)c1cccnc1
Cl-[C;H0;D3;+0:1]1=[C:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6]-[C:7]-1-[C:8].[#7;a:9]:[c:10]:[c:11]-[C:12](=[O;D1;H0:13])-[OH;D1;+0:14]>>[#7;a:9]:[c:10]:[c:11]-[C:12](=[O;D1;H0:13])-[O;H0;D2;+0:14]-[C;H0;D3;+0:1]1=[C:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6]-[C:7]-1-[C:8]
null
[]
null
null
null
null
A mixture of 200 mg (1.15 mmol) of 4-chlorobicyclo[3.2.1]oct-3-en-2-one, (Preparation Example P2) 16 mg (0.12 mmol) of ZnCl2, 324 mg (1.15 mmol) of 2-methoxyethoxymethyl-6 -trifluoromethylnicotinic acid, 166 mg (1.27 mmol) of diisopropylethylamine and 5 ml of toluene is stirred under a nitrogen atmosphere at room tempe...
10.6084/m9.figshare.5104873.v1
null
Alkenyl halide.Carboxylic acid
Ester
C1=CC2CCC(C1)C2
C1=CC2CCC(C1)C2
c1ccncc1.C1=CC2CCC(C1)C2
HCl
[Cl-].[Cl-].[Zn+2].ClCCl
null
null
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Cl)C2CCC1C2>[Cl-].[Cl-].[Zn+2].ClCCl>COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)C2CCC1C2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-409d008ed9254c7a90cc86e77c706786
O=C(O)c1ccc(Cl)cc1.O=C1C=C(Cl)C2CCC1C2>>O=C(OC1=CC(=O)C2CCC1C2)c1ccc(Cl)cc1
C1(=CC=CC=C1)C.ClC1=CC(C2CCC1C2)=O.ClC1=CC=C(C(=O)O)C=C1.C(C)(C)N(CC)C(C)C>>ClC1=CC=C(C=C1)C(=O)OC1=CC(C2CCC1C2)=O
[O:1]=[C:2]([OH:3])[c:13]1[cH:14][cH:15][c:16]([Cl:17])[cH:18][cH:19]1.Cl[C:4]1=[CH:5][C:6](=[O:7])[CH:8]2[CH2:9][CH2:10][CH:11]1[CH2:12]2>>[O:1]=[C:2]([O:3][C:4]1=[CH:5][C:6](=[O:7])[CH:8]2[CH2:9][CH2:10][CH:11]1[CH2:12]2)[c:13]1[cH:14][cH:15][c:16]([Cl:17])[cH:18][cH:19]1
O=C(O)c1ccc(Cl)cc1.O=C1C=C(Cl)C2CCC1C2
O=C(OC1=CC(=O)C2CCC1C2)c1ccc(Cl)cc1
null
[Cl-].[Cl-].[Zn+2]
ClCCl
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
b0cc2671c5188ff45d2dc8f6f4a2748058b058251e35db4909cb7151f9e28dbd
83fa46670fde4697f2da46ad00486528b93f00a3ef192db8e938bfe22fc495ff
O=C(OC1=CC(=O)C2CCC1C2)c1ccccc1
Cl-[C;H0;D3;+0:1]1=[C:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6]-[C:7]-1-[C:8].[O;D1;H0:9]=[C:10](-[OH;D1;+0:11])-[c:12]>>[C:8]-[C:7]1-[C:6]-[C:5]-[C:3](=[O;D1;H0:4])-[C:2]=[C;H0;D3;+0:1]-1-[O;H0;D2;+0:11]-[C:10](=[O;D1;H0:9])-[c:12]
84.9
[{"value": 84.9, "product": "ClC1=CC=C(C=C1)C(=O)OC1=CC(C2CCC1C2)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 500 mg of 4-chlorobicyclo[3.2.1]oct-3-en-2-one (Preparation Example P2), 440 mg of ZnCl2, 400 mg of 4-chlorobenzoic acid, 1.05 g of diisopropylethylamine and 5 ml of toluene is stirred at room temperature under a nitrogen atmosphere at reflux temperature for 6 hours. After cooling, the reaction mixture is ...
10.6084/m9.figshare.5104873.v1
null
Alkenyl halide.Carboxylic acid
Ester
C1=CC2CCC(C1)C2
C1=CC2CCC(C1)C2
C1=CC2CCC(C1)C2.c1ccccc1
HCl
[Cl-].[Cl-].[Zn+2].ClCCl
null
null
O=C(O)c1ccc(Cl)cc1.O=C1C=C(Cl)C2CCC1C2>[Cl-].[Cl-].[Zn+2].ClCCl>O=C(OC1=CC(=O)C2CCC1C2)c1ccc(Cl)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-490092c910054855818fdd351ad58b33
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Br)C2CCC1C2>>COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)C2CCC1C2
COCCOCC1=C(C(=O)O)C=CC(=N1)C(F)(F)F.CCN(C(C)C)C(C)C.COCCOCC1=C(C(=O)O)C=CC(=N1)C(F)(F)F.CCN(C(C)C)C(C)C.BrC1=CC(C2CCC1C2)=O>>COCCOCC1=NC(=CC=C1C(=O)OC1=CC(C2CCC1C2)=O)C(F)(F)F
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][c:7]1[n:8][c:9]([C:10]([F:11])([F:12])[F:13])[cH:14][cH:15][c:16]1[C:17](=[O:18])[OH:19].Br[C:20]1=[CH:21][C:22](=[O:23])[CH:24]2[CH2:25][CH2:26][CH:27]1[CH2:28]2>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][c:7]1[n:8][c:9]([C:10]([F:11])([F:12])[F:13])[cH:14][cH:15][c:16]1[C:17](=[O:1...
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Br)C2CCC1C2
COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)C2CCC1C2
null
[Cl-].[Cl-].[Zn+2].[Cl-].[Cl-].[Zn+2]
ClC1=CC=CC=C1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
b0cc2671c5188ff45d2dc8f6f4a2748058b058251e35db4909cb7151f9e28dbd
83fa46670fde4697f2da46ad00486528b93f00a3ef192db8e938bfe22fc495ff
O=C(OC1=CC(=O)C2CCC1C2)c1cccnc1
Br-[C;H0;D3;+0:1]1=[C:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6]-[C:7]-1-[C:8].[#7;a:9]:[c:10]:[c:11]-[C:12](=[O;D1;H0:13])-[OH;D1;+0:14]>>[#7;a:9]:[c:10]:[c:11]-[C:12](=[O;D1;H0:13])-[O;H0;D2;+0:14]-[C;H0;D3;+0:1]1=[C:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6]-[C:7]-1-[C:8]
null
[]
null
null
null
null
A mixture of 27 g of a 6.2% solution of 4-bromobicyclo[3.2.1]oct-3-en-2-one (Preparation Example P1) in chlorobenzene, 110 mg of ZnCl2, 2.34 g of 2-methoxyethoxymethyl-6-trifluoromethylnicotinic acid and 1.2 g of Hünig's base is stirred at room temperature under a nitrogen atmosphere until a dark-brown solution is form...
10.6084/m9.figshare.5104873.v1
null
Alkenyl halide.Carboxylic acid
Ester
C1=CC2CCC(C1)C2
C1=CC2CCC(C1)C2
c1ccncc1.C1=CC2CCC(C1)C2
HBr
[Cl-].[Cl-].[Zn+2].[Cl-].[Cl-].[Zn+2].ClC1=CC=CC=C1
null
null
COCCOCc1nc(C(F)(F)F)ccc1C(=O)O.O=C1C=C(Br)C2CCC1C2>[Cl-].[Cl-].[Zn+2].[Cl-].[Cl-].[Zn+2].ClC1=CC=CC=C1>COCCOCc1nc(C(F)(F)F)ccc1C(=O)OC1=CC(=O)C2CCC1C2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a2addf944a834de8a9024e8dbef1406e
C[C@H]1C(S(=O)(=O)c2ccccc2)C=C(Sc2ccccc2)CC[C@H]1O[Si](C)(C)C>>C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O
CO.CCN(CC)CC.C1(=CC=CC=C1)S(=O)(=O)C1[C@@H]([C@@H](CCC(=C1)SC1=CC=CC=C1)O[Si](C)(C)C)C.[Si](C)(C)(C)OS(=O)(=O)C(F)(F)F>>C[C@@H]1[C@@H](CC=C(C=C1)SC1=CC=CC=C1)O
C[Si](C)(C)[O:16][C@H:15]1[C@@H:2]([CH3:1])[CH:3](S(=O)(=O)c2ccccc2)[CH:4]=[C:5]([S:6][c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[CH2:13][CH2:14]1>>[CH3:1][C@H:2]1[CH:3]=[CH:4][C:5]([S:6][c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)=[CH:13][CH2:14][C@H:15]1[OH:16]
C[C@H]1C(S(=O)(=O)c2ccccc2)C=C(Sc2ccccc2)CC[C@H]1O[Si](C)(C)C
C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O
null
null
C(Cl)Cl.CCOC(=O)C
Functional Group Interconversion
OtherReaction
c5a8179abb456fc1073dcc1b69f4dd6858023288e1c82295e0fa28ad8154fde5
b6232982cc0a6eaeb0e19aa9e067e5a44b4ff6428382e09578f8d924ae232629
C1=CC(Sc2ccccc2)=CCCC1
C-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2]1-[C:3]-[CH2;D2;+0:4]-[C;H0;D3;+0:5](-[#16:6]-[c:7])=[CH;D2;+0:8]-[CH;D3;+0:9](-S(=O)(=O)-c2:c:c:c:c:c:2)-[C:10]-1-[C;D1;H3:11]>>[C;D1;H3:11]-[C:10]1-[CH;D2;+0:9]=[CH;D2;+0:8]-[C;H0;D3;+0:5](-[#16:6]-[c:7])=[CH;D2;+0:4]-[C:3]-[C:2]-1-[OH;D1;+0:1]
86.8
[{"value": 86.0, "product": "C[C@@H]1[C@@H](CC=C(C=C1)SC1=CC=CC=C1)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.8, "product": "C[C@@H]1[C@@H](CC=C(C=C1)SC1=CC=CC=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
8
HOUR
22 or 23 (2.15 g, 4.81 mmol) was dissolved in dry methylene chloride (20 mL), and 4.0 mL of Et3N (28.7 mmol) was added at room temperature, followed by addition of 3.0 mL (16.6 mmol) of TMSOTf. This mixture was brought to reflux under N2, and stirred for 8 h until the starting material was consumed (monitored by TLC us...
10.6084/m9.figshare.5104873.v1
null
Monosulfide.Sulfone.Silyl protective group
Secondary alcohol.Monosulfide
C1=CCCCCC1.c1ccccc1
C1=CCCCC=C1
C1=CCCCC=C1.c1ccccc1
HO-
C(Cl)Cl.CCOC(=O)C
0
8
C[C@H]1C(S(=O)(=O)c2ccccc2)C=C(Sc2ccccc2)CC[C@H]1O[Si](C)(C)C>C(Cl)Cl.CCOC(=O)C>C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-336aa01dbe29406f86a022344008d3f8
CI.C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O>>C[C@H]1C=CC(Sc2ccccc2)=C[C@H](C)[C@H]1O
C[C@@H]1[C@@H](CC=C(C=C1)SC1=CC=CC=C1)O.CI.[Li]CCCC>>C[C@@H]1[C@H]([C@H](C=CC(=C1)SC1=CC=CC=C1)C)O
I[CH3:15].[CH3:1][C@H:2]1[CH:3]=[CH:4][C:5]([S:6][c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)=[CH:13][CH2:14][C@H:16]1[OH:17]>>[CH3:1][C@H:2]1[CH:3]=[CH:4][C:5]([S:6][c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)=[CH:13][C@H:14]([CH3:15])[C@H:16]1[OH:17]
CI.C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O
C[C@H]1C=CC(Sc2ccccc2)=C[C@H](C)[C@H]1O
null
null
C1CCOC1
C-C Coupling
Methylation with MeI_secondary
21b917c068b9b7d2a61c0af1aace99f1a5bedcf90946eeff3fd7449263787c71
410ec9b1cc243569e4ff568c248f0b402403802e002b4018f576af3f6960507b
C1=CC(Sc2ccccc2)=CCCC1
I-[CH3;D1;+0:1].[#16:2]-[C:3]1=[C:4]-[CH2;D2;+0:5]-[C:6](-[O;D1;H1:7])-[C:8]-[C:9]=[C:10]-1>>[#16:2]-[C:3]1=[C:4]-[C@H;D3;+0:5](-[CH3;D1;+0:1])-[C:6](-[O;D1;H1:7])-[C:8]-[C:9]=[C:10]-1
70.1
[{"value": 70.0, "product": "C[C@@H]1[C@H]([C@H](C=CC(=C1)SC1=CC=CC=C1)C)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 70.1, "product": "C[C@@H]1[C@H]([C@H](C=CC(=C1)SC1=CC=CC=C1)C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-100
CELSIUS
1
HOUR
A solution of alcohol 29 (887 mg, 3.82 mmol) in THF (50 mL) was cooled to −78° C., and 3.20 mL of n-BuLi (2.5 M in hexanes, 8.00 mmol) was added dropwise. The mixture was slowly brought to −7° C. over 1 h, and stirred at this temperature for 10 min. It was then cooled to −100° C. in a THF-liquid N2 bath. To this cold d...
10.6084/m9.figshare.5104873.v1
null
null
null
C1=CCCCC=C1
C1=CCCCC=C1
C1=CCCCC=C1.c1ccccc1
HI
C1CCOC1
-100
1
CI.C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O>C1CCOC1>C[C@H]1C=CC(Sc2ccccc2)=C[C@H](C)[C@H]1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-1c02daaec61d4b3cbef197317b0fd01b
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O>>C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
CO.C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H](C=C1)C)O)C.N1=C(C=CC=C1C)C.[Si](C)(C)(C(C)(C)C)OS(=O)(=O)C(F)(F)F>>C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H](C=C1)C)O[Si](C)(C)C(C)(C)C)C
O=S(=O)(O[Si:20]([CH3:21])([CH3:22])[C:23]([CH3:24])([CH3:25])[CH3:26])C(F)(F)F.[CH3:1][C@H:2]1[CH:3]=[CH:4][C:5]([S:6](=[O:7])(=[O:8])[c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)=[CH:15][C@H:16]([CH3:17])[C@H:18]1[OH:19]>>[CH3:1][C@H:2]1[CH:3]=[CH:4][C:5]([S:6](=[O:7])(=[O:8])[c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)...
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O
C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
null
null
C(Cl)Cl
Functional Group Interconversion
OtherReaction
5538bfc5ecbe9cd9a5fd4ec1ef8ed524aca8f082f4aad29482d3c63cae96472f
55a582b0275cf25a85be636ee06e566428dd16a5bf0128e091e139c3b4d668ec
O=S(=O)(C1=CCCCC=C1)c1ccccc1
F-C(-F)(-F)-S(=O)(=O)-O-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7].[OH;D1;+0:8]-[C:9]1-[C:10]-[C:11]=[C:12]-[C:13]=[C:14]-[C:15]-1>>[C;D1;H3:2]-[Si;H0;D4;+0:1](-[C;D1;H3:3])(-[O;H0;D2;+0:8]-[C:9]1-[C:10]-[C:11]=[C:12]-[C:13]=[C:14]-[C:15]-1)-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6...
98
[{"value": 98.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H](C=C1)C)O[Si](C)(C)C(C)(C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.8, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H](C=C1)C)O[Si](C)(C)C(C)(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
A solution of alcohol 32 (550 mg, 1.98 mmol) and 2,6-lutidine (0.34 mL, 2.97 mmol) in CH2Cl2 (20 mL) was cooled to −78° C., and 0.55 mL (2.39 mmol) of TBSOTf was added. The cold solution was stirred and allowed to warm to 0° C. over a 1 h. MeOH (40 μL, 1 mmol) was then added and the resulting mixture was concentrated v...
10.6084/m9.figshare.5104873.v1
null
Triflate.Secondary alcohol.TMS ether protective group
TMS ether protective group
null
null
C1=CCCCC=C1.c1ccccc1
TfOH.HO-
C(Cl)Cl
0
null
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O>C(Cl)Cl>C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-f7b1fcffd58148b790e375925e1c0e94
CC=[N+]=CC.C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O>>C[C@H]1C=CC(Sc2ccccc2)=C[C@H](CN(C)C)[C@H]1O
C(=O)(O)[O-].[Na+].[Li]CCCC.C[C@@H]1[C@@H](CC=C(C=C1)SC1=CC=CC=C1)O.[I-].CC=[N+]=CC>>CN(C)C[C@@H]1[C@H]([C@H](C=CC(=C1)SC1=CC=CC=C1)C)O
C[CH:15]=[N+:16]=[CH:17][CH3:18].[CH3:1][C@H:2]1[CH:3]=[CH:4][C:5]([S:6][c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)=[CH:13][CH2:14][C@H:19]1[OH:20]>>[CH3:1][C@H:2]1[CH:3]=[CH:4][C:5]([S:6][c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)=[CH:13][C@H:14]([CH2:15][N:16]([CH3:17])[CH3:18])[C@H:19]1[OH:20]
CC=[N+]=CC.C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O
C[C@H]1C=CC(Sc2ccccc2)=C[C@H](CN(C)C)[C@H]1O
null
null
C(Cl)Cl.CO.C1CCOC1
Functional Group Addition
OtherReaction
1c8bd53765008786c2e459063d4bf8e8a6b2967c8a491a3b9823c42d8b3faebb
a5ecc0f9f40a26873e3f25b9146fa7daf7ef454ae1fed653ab37babf6624d21a
C1=CC(Sc2ccccc2)=CCCC1
C-[CH;D2;+0:1]=[N+;H0;D2:2]=[CH;D2;+0:3]-[CH3;D1;+0:4].[#16:5]-[C:6]1=[C:7]-[CH2;D2;+0:8]-[C:9](-[O;D1;H1:10])-[C:11]-[C:12]=[C:13]-1>>[#16:5]-[C:6]1=[C:7]-[C@H;D3;+0:8](-[CH2;D2;+0:1]-[N;H0;D3;+0:2](-[CH3;D1;+0:3])-[CH3;D1;+0:4])-[C:9](-[O;D1;H1:10])-[C:11]-[C:12]=[C:13]-1
58
[{"value": 58.0, "product": "CN(C)C[C@@H]1[C@H]([C@H](C=CC(=C1)SC1=CC=CC=C1)C)O", "details": "PERCENTYIELD", "is_desired": false}]
-7
CELSIUS
1
HOUR
A solution of alcohol 29 (80 mg, 0.34 mmol) in THF (4 mL) was cooled to −78° C., and 0.30 mL of n-BuLi (2.5M in hexanes, 0.75 mmol) was added dropwise via syringe. This mixture was brought to −7° C. over 1 h, and stirred at −7° C. for 10 min, then cooled to −78° C., and transferred to a flask containing N,N-dimethylmet...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amine
C1=CCCCC=C1
C1=CCCCC=C1
C1=CCCCC=C1.c1ccccc1
Other
C(Cl)Cl.CO.C1CCOC1
-7
1
CC=[N+]=CC.C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O>C(Cl)Cl.CO.C1CCOC1>C[C@H]1C=CC(Sc2ccccc2)=C[C@H](CN(C)C)[C@H]1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b21ca584e8cd4b3989e87ac2851e83ab
C[C@H]1C=CC(Sc2ccccc2)=C[C@H](CN(C)C)[C@H]1O.O=C(OO)c1cccc(Cl)c1>>C=C1C=C(S(=O)(=O)c2ccccc2)C=C[C@H](C)[C@@H]1O
OS(=O)[O-].[Na+].CN(C)C[C@@H]1[C@H]([C@H](C=CC(=C1)SC1=CC=CC=C1)C)O.C1=CC(=CC(=C1)Cl)C(=O)OO>>C1(=CC=CC=C1)S(=O)(=O)C1=CC([C@H]([C@H](C=C1)C)O)=C
CN(C)[CH2:1][C@H:2]1[CH:3]=[C:4]([S:5][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[CH:14]=[CH:15][C@H:16]([CH3:17])[C@@H:18]1[OH:19].OOC(c1cccc(Cl)c1)=[O:6]>>[CH2:1]=[C:2]1[CH:3]=[C:4]([S:5](=[O:6])(=[O:7])[c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[CH:14]=[CH:15][C@H:16]([CH3:17])[C@@H:18]1[OH:19]
C[C@H]1C=CC(Sc2ccccc2)=C[C@H](CN(C)C)[C@H]1O.O=C(OO)c1cccc(Cl)c1
C=C1C=C(S(=O)(=O)c2ccccc2)C=C[C@H](C)[C@@H]1O
null
null
C(Cl)Cl
Oxidation
OtherReaction
4e73d8a6e53dce15b599fa81e988dc52b98d89f1f1c66213112ad885558686e7
f575dc3da217eae1ac1d3f527627a065b02dc653aa7aedb45e854bbd5e8c558c
C=C1C=C(S(=O)(=O)c2ccccc2)C=CCC1
C-N(-C)-[CH2;D2;+0:1]-[C@H;D3;+0:2]1-[C:3]=[C:4](-[S;H0;D2;+0:5]-[c:6](:[c:7]):[c:8])-[C:9]=[C:10]-[C:11]-[C:12]-1-[O;D1;H1:13].Cl-c1:c:c:c:c(-C(=[O;H0;D1;+0:14])-O-O):c:1>>[CH2;D1;+0:1]=[C;H0;D3;+0:2]1-[C:3]=[C:4](-[S;H0;D4;+0:5](=[O;D1;H0:15])(=[O;H0;D1;+0:14])-[c:6](:[c:7]):[c:8])-[C:9]=[C:10]-[C:11]-[C:12]-1-[O;D1;...
null
[]
null
null
30
MINUTE
To a solution of amine 34 (42 mg, 0.14 mmol) in CH2Cl2 (2 mL) was added 140 mg of m-CPBA (0.57 mmol based on 70% content). The mixture was stirred at room temperature for 30 min, then aqueous NaHSO3 was added, the resulting two layers were separated, and the aqueous phase was extracted with CH2Cl2 (3×3 mL). The combine...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tertiary amine.Peroxide.Monosulfide
Sulfone.Vinyl
C1=CCCCC=C1.c1ccccc1
C1=CCCCC=C1
C1=CCCCC=C1.c1ccccc1
HCl
C(Cl)Cl
null
0.5
C[C@H]1C=CC(Sc2ccccc2)=C[C@H](CN(C)C)[C@H]1O.O=C(OO)c1cccc(Cl)c1>C(Cl)Cl>C=C1C=C(S(=O)(=O)c2ccccc2)C=C[C@H](C)[C@@H]1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-86f49c24746b4b3a8725423ba5400fa9
CC(C)(C)OO.C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O>>C[C@@H]1[C@H](O)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)[C@@H]2O[C@H]12
C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H](C=C1)C)O)C.C(C)(C)(C)OO>>C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@H]2O[C@@H]12)C)O)C
CC(C)(C)O[OH:19].[CH3:1][C@@H:2]1[C@@H:3]([OH:4])[C@@H:5]([CH3:6])[CH:7]=[CH:18][C:8]([S:9](=[O:10])(=[O:11])[c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)=[CH:20]1>>[CH3:1][C@@H:2]1[C@H:3]([OH:4])[C@@H:5]([CH3:6])[CH:7]=[C:8]([S:9](=[O:10])(=[O:11])[c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[C@@H:18]2[O:19][C@H:20]12
CC(C)(C)OO.C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O
C[C@@H]1[C@H](O)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)[C@@H]2O[C@H]12
null
[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[Mo]
C1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
eea2dab1111e082cf7b8c07a2e45ffe4ee54f851a6b2dc0700e3bea011267548
42a03c3e3056d859131de561fc8292c06b2910df7e46ddbdd3187d6cec35220b
O=S(=O)(C1=CCCC[C@H]2O[C@@H]12)c1ccccc1
C-C(-C)(-C)-O-[OH;D1;+0:1].[C;D1;H3:2]-[C:3]1-[C:4]-[C:5](-[C;D1;H3:6])-[CH;D2;+0:7]=[CH;D2;+0:8]-[C;H0;D3;+0:9](-[#16:10](=[O;D1;H0:11])(=[O;D1;H0:12])-[c:13])=[CH;D2;+0:14]-1>>[C;D1;H3:2]-[C:3]1-[C:4]-[C:5](-[C;D1;H3:6])-[CH;D2;+0:7]=[C;H0;D3;+0:9](-[#16:10](=[O;D1;H0:11])(=[O;D1;H0:12])-[c:13])-[C@@H;D3;+0:8]2-[O;H0...
88
[{"value": 88.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@H]2O[C@@H]12)C)O)C", "details": "PERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
A suspension of dienyl sulfone 32 (67 mg, 0.24 mmol), molybdenum hexacarbonyl (3 mg, 0.01 mmol), and tert-butylhydroperoxide (74 μL of 5M solution in decane) in benzene (3 mL) was heated at 80° C. for 10 h. The reaction mixture was concentrated via rotary evaporation, purified by flash column chromatography (ethyl acet...
10.6084/m9.figshare.5104873.v1
null
Peroxide
Ether
C1=CCCCC=C1
C1=C[C@@H]2O[C@@H]2CCC1
c1ccccc1.C1=C[C@@H]2O[C@@H]2CCC1
HO-
[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[Mo].C1=CC=CC=C1
80
null
CC(C)(C)OO.C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O>[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[Mo].C1=CC=CC=C1>C[C@@H]1[C@H](O)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)[C@@H]2O[C@H]12
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-7062d2f0602944bcae3a395bd632b80a
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@@H]1[C@H](O)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)[C@@H]2O[C@H]12>>C[C@H]1[C@H]2O[C@H]2C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
CO.C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@H]2O[C@@H]12)C)O)C.N1=C(C=CC=C1C)C.[Si](C)(C)(C(C)(C)C)OS(=O)(=O)C(F)(F)F>>C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@H]2O[C@@H]12)C)O[Si](C)(C)C(C)(C)C)C
O=S(=O)(O[Si:21]([CH3:22])([CH3:23])[C:24]([CH3:25])([CH3:26])[CH3:27])C(F)(F)F.[CH3:1][C@H:2]1[C@H:3]2[O:4][C@H:5]2[C:6]([S:7](=[O:8])(=[O:9])[c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)=[CH:16][C@H:17]([CH3:18])[C@H:19]1[OH:20]>>[CH3:1][C@H:2]1[C@H:3]2[O:4][C@H:5]2[C:6]([S:7](=[O:8])(=[O:9])[c:10]2[cH:11][cH:12][cH:1...
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@@H]1[C@H](O)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)[C@@H]2O[C@H]12
C[C@H]1[C@H]2O[C@H]2C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
null
null
C(Cl)Cl
Functional Group Interconversion
OtherReaction
5538bfc5ecbe9cd9a5fd4ec1ef8ed524aca8f082f4aad29482d3c63cae96472f
55a582b0275cf25a85be636ee06e566428dd16a5bf0128e091e139c3b4d668ec
O=S(=O)(C1=CCCC[C@H]2O[C@@H]12)c1ccccc1
F-C(-F)(-F)-S(=O)(=O)-O-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7].[C:8]-[C:9](-[OH;D1;+0:10])-[C:11]-[C:12]=[C:13]>>[C:8]-[C:9](-[O;H0;D2;+0:10]-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7])-[C:11]-[C:12]=[C:13]
95.6
[{"value": 95.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@H]2O[C@@H]12)C)O[Si](C)(C)C(C)(C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.6, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@H]2O[C@@H]12)C)O[Si](C)(C)C(C)(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is...
-78
CELSIUS
null
null
A mixture of alcohol α36 (62 mg, 0.21 mmol) and 2,6-lutidine (50 μL, 0.43 mmol) in CH2Cl2 (2 mL) was cooled to −78° C., and 63 μL (0.27 mmol) of TBSOTf was added. The stirred cold solution was warmed to 0° C. over 5 h. MeOH (40 μL, 1 mmol) was then added to quench the excess TBSOTf. The resulting mixture was concentrat...
10.6084/m9.figshare.5104873.v1
null
Triflate.Secondary alcohol.TMS ether protective group
TMS ether protective group
null
null
C1=C[C@@H]2O[C@@H]2CCC1.c1ccccc1
TfOH.HO-
C(Cl)Cl
-78
null
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@@H]1[C@H](O)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)[C@@H]2O[C@H]12>C(Cl)Cl>C[C@H]1[C@H]2O[C@H]2C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-978d8844d75b40e69912f3415fd0a03e
C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C>>C[C@H]1[C@H](O)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H](C=C1)C)O[Si](C)(C)C(C)(C)C)C.C[N+]1(CCOCC1)[O-].[O-]S(=O)(=S)[O-].[Na+].[Na+]>>C1(=CC=CC=C1)S(=O)(=O)C=1[C@H]([C@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O)O
[CH3:1][C@H:2]1[CH:3]=[CH:5][C:7]([S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)=[CH:17][C@H:18]([CH3:19])[C@H:20]1[O:21][Si:22]([CH3:23])([CH3:24])[C:25]([CH3:26])([CH3:27])[CH3:28]>>[CH3:1][C@H:2]1[C@H:3]([OH:4])[C@H:5]([OH:6])[C:7]([S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2...
C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
C[C@H]1[C@H](O)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
null
O=[Os](=O)(=O)=O
O.CC(=O)C.C(C)(=O)OCC
Oxidation
Alkene to diol
7e69a9bdf93826c76ddd41cc5796f4a45c5625e9ad9b7072dbd7eeda89cd597d
4ce7d04b0dc7802a0fb0fdf6618787b32ab28eb210bbbb25767ced5b1fe9204d
O=S(=O)(C1=CCCCCC1)c1ccccc1
[#16:1]-[C:2]1=[C:3]-[C:4]-[C:5]-[C:6](-[C;D1;H3:7])-[CH;D2;+0:8]=[CH;D2;+0:9]-1>>[#16:1]-[C:2]1=[C:3]-[C:4]-[C:5]-[C:6](-[C;D1;H3:7])-[C@H;D3;+0:8](-[O;D1;H1:10])-[C@@H;D3;+0:9]-1-[O;D1;H1:11]
83
[{"value": 83.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C=1[C@H]([C@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
36
HOUR
A mixture of dienyl sulfone 33 (45 mg, 0.11 mmol), OsO4 (2 mg, 0.0078 mmol), 4-methylmorpholine N-oxide (27 mg, 0.23 mmol) in acetone (0.5 mL) and H2O (0.5 mL) as co-solvent was stirred at room temperature for 36 h, then saturated aqueous Na2S2O3 (5 mL) was added, and stirred for 30 min. The reaction mixture was dilute...
10.6084/m9.figshare.5104873.v1
null
null
Secondary alcohol.Secondary alcohol
C1=CCCCC=C1
C1=CCCCCC1
C1=CCCCCC1.c1ccccc1
Other
O=[Os](=O)(=O)=O.O.CC(=O)C.C(C)(=O)OCC
null
36
C[C@H]1C=CC(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C>O=[Os](=O)(=O)=O.O.CC(=O)C.C(C)(=O)OCC>C[C@H]1[C@H](O)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-7137800094964e29955ab14be3d26d96
CC(=O)OC(C)=O.C[C@@H]1[C@H](O)CCC(Sc2ccccc2)=C[C@@H]1S(=O)(=O)c1ccccc1>>CC(=O)O[C@H]1CCC(=O)C[C@@H](S(=O)(=O)c2ccccc2)[C@H]1C
C1(=CC=CC=C1)S(=O)(=O)[C@@H]1[C@@H]([C@@H](CCC(=C1)SC1=CC=CC=C1)O)C.C(C)(=O)OC(C)=O.C(C)N(CC)CC.[I-].[Na+].Cl[Si](C)(C)C.O.C1(=CC=CC=C1)S(=O)(=O)[C@@H]1[C@@H]([C@@H](CCC(=C1)SC1=CC=CC=C1)O)C>>C1(=CC=CC=C1)S(=O)(=O)[C@H]1[C@H]([C@H](CCC(C1)=O)OC(C)=O)C
CC(O[C:2]([CH3:1])=[O:3])=[O:9].c1ccc(S[C:8]2=[CH:10][C@H:11]([S:12](=[O:13])(=[O:14])[c:15]3[cH:16][cH:17][cH:18][cH:19][cH:20]3)[C@H:21]([CH3:22])[C@H:5]([OH:4])[CH2:6][CH2:7]2)cc1>>[CH3:1][C:2](=[O:3])[O:4][C@H:5]1[CH2:6][CH2:7][C:8](=[O:9])[CH2:10][C@@H:11]([S:12](=[O:13])(=[O:14])[c:15]2[cH:16][cH:17][cH:18][cH:19...
CC(=O)OC(C)=O.C[C@@H]1[C@H](O)CCC(Sc2ccccc2)=C[C@@H]1S(=O)(=O)c1ccccc1
CC(=O)O[C@H]1CCC(=O)C[C@@H](S(=O)(=O)c2ccccc2)[C@H]1C
null
Cl[Hg]Cl
ClCCl.C(C)#N
Acylation
OtherReaction
8b047b910960ca5036329fbb60c10d38c50df9fd85dbfacaf84dc2f8c120600c
295c5e035c2f8a1953383ce9322128b08edd510507adc4edb1b31e2c834ae9cf
O=C1CCCC[C@H](S(=O)(=O)c2ccccc2)C1
C-C(=[O;H0;D1;+0:1])-O-[C;H0;D3;+0:2](-[C;D1;H3:3])=[O;D1;H0:4].[#16:5]-[C:6]1-[C:7]-[C:8](-[OH;D1;+0:9])-[C:10]-[C:11]-[C;H0;D3;+0:12](-S-c2:c:c:c:c:c:2)=[CH;D2;+0:13]-1>>[#16:5]-[C:6]1-[C:7]-[C:8](-[O;H0;D2;+0:9]-[C;H0;D3;+0:2](-[C;D1;H3:3])=[O;D1;H0:4])-[C:10]-[C:11]-[C;H0;D3;+0:12](=[O;H0;D1;+0:1])-[CH2;D2;+0:13]-1
85
[{"value": 85.0, "product": "C1(=CC=CC=C1)S(=O)(=O)[C@H]1[C@H]([C@H](CCC(C1)=O)OC(C)=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.9, "product": "C1(=CC=CC=C1)S(=O)(=O)[C@H]1[C@H]([C@H](CCC(C1)=O)OC(C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 21 (4.63 g, 12.38 mmol) in dichloromethane (62 mL) was added acetic anhydride (1.40 mL, 14.9 mmol), triethylamine (2.61 mL, 18.6 mmol), and a catalytic amount of N,N-dimethylaminopyridine. The solution was stirred for 30 minutes at room temperature, diluted with dichloromethane (60 mL), washed with wat...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Secondary alcohol.Monosulfide
Ketone.Ester
c1ccccc1.C1=CCCCCC1
C1CCCCCC1
C1CCCCCC1.c1ccccc1
Other
Cl[Hg]Cl.ClCCl.C(C)#N
null
0.5
CC(=O)OC(C)=O.C[C@@H]1[C@H](O)CCC(Sc2ccccc2)=C[C@@H]1S(=O)(=O)c1ccccc1>Cl[Hg]Cl.ClCCl.C(C)#N>CC(=O)O[C@H]1CCC(=O)C[C@@H](S(=O)(=O)c2ccccc2)[C@H]1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-39222e8f250c4a279aec2e928411e88c
C[C@H]1[C@H]2O[C@H]2C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C>>C[C@@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)C[C@@H]1O
C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@H]2O[C@@H]12)C)O[Si](C)(C)C(C)(C)C)C.C1CCOC1.CC(C)C[AlH]CC(C)C>>C1(=CC=CC=C1)S(=O)(=O)C=1C[C@@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O
[CH3:1][C@@H:2]1[C@H:3]([O:4][Si:5]([CH3:6])([CH3:7])[C:8]([CH3:9])([CH3:10])[CH3:11])[C@@H:12]([CH3:13])[CH:14]=[C:15]([S:16](=[O:17])(=[O:18])[c:19]2[cH:20][cH:21][cH:22][cH:23][cH:24]2)[C@H:25]2[C@@H:26]1[O:27]2>>[CH3:1][C@@H:2]1[C@H:3]([O:4][Si:5]([CH3:6])([CH3:7])[C:8]([CH3:9])([CH3:10])[CH3:11])[C@@H:12]([CH3:13]...
C[C@H]1[C@H]2O[C@H]2C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
C[C@@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)C[C@@H]1O
null
null
C1(=CC=CC=C1)C
Reduction
OtherReaction
074bf371dcb142f3532dac755d4497500a2fbf5507a41d6c839926a966132f47
7198fae1b68de0a7b3cad42fd2e176cc1d426019158d5ea9d2333b476668381b
O=S(=O)(C1=CCCCCC1)c1ccccc1
[#16:1]-[C:2]1=[C:3]-[C:4]-[C:5]-[C:6](-[C;D1;H3:7])-[C@H;D3;+0:8]2-[O;H0;D2;+0:9]-[C@@H;D3;+0:10]-1-2>>[#16:1]-[C:2]1=[C:3]-[C:4]-[C:5]-[C:6](-[C;D1;H3:7])-[C@@H;D3;+0:8](-[OH;D1;+0:9])-[CH2;D2;+0:10]-1
87.2
[{"value": 85.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C=1C[C@@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.2, "product": "C1(=CC=CC=C1)S(=O)(=O)C=1C[C@@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O", "details": "CALCULATEDPERCENTYIELD", "is_desir...
-78
CELSIUS
3
HOUR
Compound α37 (39 mg, 0.095 mmol) was dissolved in dry toluene (1.0 mL), and the temperature lowered to −78° C. To this cold solution was added THF (10 μL, 0.12 mmol), followed by DIBAL-H solution (0.20 mL of 1.55M in toluene) under nitrogen, and the reaction stirred magnetically at −78° C. for 3 hours. Upon completion,...
10.6084/m9.figshare.5104873.v1
null
Ether
Secondary alcohol
C1=C[C@@H]2O[C@@H]2CCC1
C1=CCCCCC1
C1=CCCCCC1.c1ccccc1
null
C1(=CC=CC=C1)C
-78
3
C[C@H]1[C@H]2O[C@H]2C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C>C1(=CC=CC=C1)C>C[C@@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)C=C(S(=O)(=O)c2ccccc2)C[C@@H]1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-72bc74af69114b41ab0a74cdf3541e4c
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@H]1[C@H](O)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C>>C[C@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
C1(=CC=CC=C1)S(=O)(=O)C=1[C@H]([C@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O)O.N1=C(C=CC=C1C)C.CO.[Si](C)(C)(C(C)(C)C)OS(=O)(=O)C(F)(F)F>>C1(=CC=CC=C1)S(=O)(=O)C=1[C@H]([C@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O[Si](C)(C)C(C)(C)C)O
O=S(=O)(O[Si:5]([CH3:6])([CH3:7])[C:8]([CH3:9])([CH3:10])[CH3:11])C(F)(F)F.[CH3:1][C@H:2]1[C@H:3]([OH:4])[C@H:12]([OH:13])[C:14]([S:15](=[O:16])(=[O:17])[c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)=[CH:24][C@H:25]([CH3:26])[C@H:27]1[O:28][Si:29]([CH3:30])([CH3:31])[C:32]([CH3:33])([CH3:34])[CH3:35]>>[CH3:1][C@H:2]1[C@H...
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@H]1[C@H](O)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
C[C@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
null
null
C(Cl)Cl
Functional Group Interconversion
OtherReaction
5538bfc5ecbe9cd9a5fd4ec1ef8ed524aca8f082f4aad29482d3c63cae96472f
55a582b0275cf25a85be636ee06e566428dd16a5bf0128e091e139c3b4d668ec
O=S(=O)(C1=CCCCCC1)c1ccccc1
F-C(-F)(-F)-S(=O)(=O)-O-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7].[C:8]=[C:9]-[C:10]-[C:11](-[OH;D1;+0:12])-[C:13]>>[C:8]=[C:9]-[C:10]-[C:11](-[O;H0;D2;+0:12]-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7])-[C:13]
99.6
[{"value": 99.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C=1[C@H]([C@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O[Si](C)(C)C(C)(C)C)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.6, "product": "C1(=CC=CC=C1)S(=O)(=O)C=1[C@H]([C@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O[Si](C)(C)C(C)(C)C)O"...
-78
CELSIUS
2
HOUR
Compound 39 (77 mg, 0.18 mmol) was dissolved in dry methylene chloride (2.0 mL), and cooled to −78° C. To this cold solution were added 2,6-lutidine (32 μL, 0.27 mmol), followed by TBSOTf (50 μL, 0.22 mmol) under nitrogen. After stirring for 2 h at −78° C. (the reaction was monitored by TLC until completionusing a mixt...
10.6084/m9.figshare.5104873.v1
null
Triflate.Secondary alcohol.TMS ether protective group
TMS ether protective group
null
null
C1=CCCCCC1.c1ccccc1
TfOH.HO-
C(Cl)Cl
-78
2
CC(C)(C)[Si](C)(C)OS(=O)(=O)C(F)(F)F.C[C@H]1[C@H](O)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C>C(Cl)Cl>C[C@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b1782a0af1a84ba9b389e90c07478f26
CI.C[C@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C>>CO[C@@H]1C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)[C@@H]1O[Si](C)(C)C(C)(C)C
O.C1(=CC=CC=C1)S(=O)(=O)C=1[C@H]([C@H]([C@@H]([C@@H]([C@H](C1)C)O[Si](C)(C)C(C)(C)C)C)O[Si](C)(C)C(C)(C)C)O.CI.[OH-].[K+]>>C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@@H]([C@@H]1OC)O[Si](C)(C)C(C)(C)C)C)O[Si](C)(C)C(C)(C)C)C
I[CH3:1].[OH:2][C@@H:3]1[C:4]([S:5](=[O:6])(=[O:7])[c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)=[CH:14][C@H:15]([CH3:16])[C@@H:17]([O:18][Si:19]([CH3:20])([CH3:21])[C:22]([CH3:23])([CH3:24])[CH3:25])[C@@H:26]([CH3:27])[C@@H:28]1[O:29][Si:30]([CH3:31])([CH3:32])[C:33]([CH3:34])([CH3:35])[CH3:36]>>[CH3:1][O:2][C@@H:3]1[C:4...
CI.C[C@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C
CO[C@@H]1C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)[C@@H]1O[Si](C)(C)C(C)(C)C
null
null
C(C)(=O)OCC.CCCCCC.CS(=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
31ec8f945a35f4f87287620e27b68692ce42732551035fbac056df61d9acce14
08f7221cae607d413f579138dcaa6997bebcad2bbb42d2f1b3b2a2d886befb37
O=S(=O)(C1=CCCCCC1)c1ccccc1
I-[CH3;D1;+0:1].[#16:2]-[C:3](=[C:4]-[C:5])-[C:6](-[OH;D1;+0:7])-[C:8]>>[#16:2]-[C:3](=[C:4]-[C:5])-[C:6](-[O;H0;D2;+0:7]-[CH3;D1;+0:1])-[C:8]
94
[{"value": 94.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@@H]([C@@H]1OC)O[Si](C)(C)C(C)(C)C)C)O[Si](C)(C)C(C)(C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.7, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@@H]([C@H]([C@H]([C@@H]([C@@H]1OC)O[Si](C)(C)C(C)(C)C)C)O[Si](C)(C)C(C)(C)C)C"...
null
null
5
MINUTE
To a solution of compound 52 (75 mg, 0.14 mmol) and MeI (86 μL, 1.4 mmol) in DMSO (2.0 mL) was added powdered KOH (23 mg, 0.42 mmol) and the resulting mixture was stirred for 5 min (until no starting material was present by TLC, developed in 1:3 EA/hexanes) at room temperature. 5 mL of H2O was added, and extracted with...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ether
null
null
C1=CCCCCC1.c1ccccc1
HI
C(C)(=O)OCC.CCCCCC.CS(=O)C
null
0.083333
CI.C[C@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@H](O)C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@H]1O[Si](C)(C)C(C)(C)C>C(C)(=O)OCC.CCCCCC.CS(=O)C>CO[C@@H]1C(S(=O)(=O)c2ccccc2)=C[C@H](C)[C@@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)[C@@H]1O[Si](C)(C)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d87b75ced07142f3b235698e7c4c8744
CC1C(O)CC=CC1S(=O)(=O)c1ccccc1>>C[C@H]1CCC(=O)C=C1S(=O)(=O)c1ccccc1
[Li]C.[NH4+].[Cl-].[Li+].C[Si](C)(C)[N-][Si](C)(C)C.C1(=CC=CC=C1)S(=O)(=O)C1C=CCC(C1C)O>>C1(=CC=CC=C1)S(=O)(=O)C1=CC(CC[C@@H]1C)=O
[CH3:1][CH:2]1[CH:3]([OH:6])[CH2:4][CH:5]=[CH:7][CH:8]1[S:9](=[O:10])(=[O:11])[c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1>>[CH3:1][C@H:2]1[CH2:3][CH2:4][C:5](=[O:6])[CH:7]=[C:8]1[S:9](=[O:10])(=[O:11])[c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1
CC1C(O)CC=CC1S(=O)(=O)c1ccccc1
C[C@H]1CCC(=O)C=C1S(=O)(=O)c1ccccc1
null
null
CCOCC.C1CCOC1
Miscellaneous
OtherReaction
53cf4e2066676acec66f9f3f7a3a23d51f563226cdd6f5b0777cb107a8e9d680
ef59ba7fad669d0d82c4daf03280dc0366c9a31cf6192836b4997e72f66f9d7c
O=C1C=C(S(=O)(=O)c2ccccc2)CCC1
[C;D1;H3:1]-[CH;D3;+0:2]1-[CH;D3;+0:3](-[OH;D1;+0:4])-[C:5]-[CH;D2;+0:6]=[CH;D2;+0:7]-[CH;D3;+0:8]-1-[#16:9](=[O;D1;H0:10])(=[O;D1;H0:11])-[c:12]>>[C;D1;H3:1]-[C@H;D3;+0:2]1-[CH2;D2;+0:3]-[C:5]-[C;H0;D3;+0:6](=[O;H0;D1;+0:4])-[CH;D2;+0:7]=[C;H0;D3;+0:8]-1-[#16:9](=[O;D1;H0:10])(=[O;D1;H0:11])-[c:12]
92
[{"value": 92.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=CC(CC[C@@H]1C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
(1S, 55, 65)-5-Benzenesulfonyl-6-methylcyclohex-3-enol (22aMe). To a solution of epoxy-dienyl sulfone SS-9a (0.377 g, 1.6 mmol) in THF (10 mL) at −78° C. was slowly added LiHMDS (1.8 mL, 1.8 mmol). The solution was stirred for 30 min, followed by addition of sat'd solution of NH4Cl (5 mL). Et2O (5 mL) was added to the ...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
C1=CCCCC1
C1=CCCCC1
C1=CCCCC1.c1ccccc1
null
CCOCC.C1CCOC1
null
0.5
CC1C(O)CC=CC1S(=O)(=O)c1ccccc1>CCOCC.C1CCOC1>C[C@H]1CCC(=O)C=C1S(=O)(=O)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-59170692a13f45e899dfc7157f96b4d9
CC(C)C1C(O)CC=CC1S(=O)(=O)c1ccccc1>>C[C@H]1CCC(=O)C=C1S(=O)(=O)c1ccccc1
[Li+].C[Si](C)(C)[N-][Si](C)(C)C.C1(=CC=CC=C1)S(=O)(=O)C1C=CCC(C1C(C)C)O.[NH4+].[Cl-].C(C)(C)[Mg]Cl>>C1(=CC=CC=C1)S(=O)(=O)C1=CC(CC[C@@H]1C)=O
C[CH:1](C)[CH:2]1[CH:3]([OH:6])[CH2:4][CH:5]=[CH:7][CH:8]1[S:9](=[O:10])(=[O:11])[c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1>>[CH3:1][C@H:2]1[CH2:3][CH2:4][C:5](=[O:6])[CH:7]=[C:8]1[S:9](=[O:10])(=[O:11])[c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1
CC(C)C1C(O)CC=CC1S(=O)(=O)c1ccccc1
C[C@H]1CCC(=O)C=C1S(=O)(=O)c1ccccc1
null
null
CCOCC.C1CCOC1
Miscellaneous
OtherReaction
53cf4e2066676acec66f9f3f7a3a23d51f563226cdd6f5b0777cb107a8e9d680
ef59ba7fad669d0d82c4daf03280dc0366c9a31cf6192836b4997e72f66f9d7c
O=C1C=C(S(=O)(=O)c2ccccc2)CCC1
C-[CH;D3;+0:1](-C)-[CH;D3;+0:2]1-[CH;D3;+0:3](-[OH;D1;+0:4])-[C:5]-[CH;D2;+0:6]=[CH;D2;+0:7]-[CH;D3;+0:8]-1-[#16:9](=[O;D1;H0:10])(=[O;D1;H0:11])-[c:12]>>[CH3;D1;+0:1]-[C@H;D3;+0:2]1-[CH2;D2;+0:3]-[C:5]-[C;H0;D3;+0:6](=[O;H0;D1;+0:4])-[CH;D2;+0:7]=[C;H0;D3;+0:8]-1-[#16:9](=[O;D1;H0:10])(=[O;D1;H0:11])-[c:12]
89
[{"value": 89.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=CC(CC[C@@H]1C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
(1S, 55, 65)-5-Benzenesulfonyl-6-methylcyclohex-3-enol (22aMe). To a solution of epoxy-dienyl sulfone SS-9a (0.377 g, 1.6 mmol) in THF (10 mL) at −78° C. was slowly added LiHMDS (1.8 mL, 1.8 mmol). The solution was stirred for 30 min, followed by addition of sat'd solution of NH4Cl (5 mL). Et2O (5 mL) was added to the ...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
C1=CCCCC1
C1=CCCCC1
C1=CCCCC1.c1ccccc1
Other
CCOCC.C1CCOC1
null
0.5
CC(C)C1C(O)CC=CC1S(=O)(=O)c1ccccc1>CCOCC.C1CCOC1>C[C@H]1CCC(=O)C=C1S(=O)(=O)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-92ca338d45f34950ac71e0f1069d5ed8
CC(C)[C@@H]1[C@@H](S(=O)(=O)c2ccccc2)[C@@H]2O[C@@H]2C[C@@H]1O[Si](C)(C)C(C)(C)C>>C[C@@H]1[C@@H](S(=O)(=O)c2ccccc2)[C@@H]2O[C@@H]2C[C@@H]1O[Si](C)(C)C(C)(C)C
C1(=CC=CC=C1)S(=O)(=O)[C@@H]1[C@H]([C@H](C[C@H]2O[C@@H]12)O[Si](C)(C)C(C)(C)C)C(C)C>>C1(=CC=CC=C1)S(=O)(=O)[C@@H]1[C@H]([C@H](C[C@H]2O[C@@H]12)O[Si](C)(C)C(C)(C)C)C
C[CH:1](C)[C@@H:2]1[C@@H:3]([S:4](=[O:5])(=[O:6])[c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[C@@H:13]2[O:14][C@@H:15]2[CH2:16][C@@H:17]1[O:18][Si:19]([CH3:20])([CH3:21])[C:22]([CH3:23])([CH3:24])[CH3:25]>>[CH3:1][C@@H:2]1[C@@H:3]([S:4](=[O:5])(=[O:6])[c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[C@@H:13]2[O:14][C@@H:15]2[CH2...
CC(C)[C@@H]1[C@@H](S(=O)(=O)c2ccccc2)[C@@H]2O[C@@H]2C[C@@H]1O[Si](C)(C)C(C)(C)C
C[C@@H]1[C@@H](S(=O)(=O)c2ccccc2)[C@@H]2O[C@@H]2C[C@@H]1O[Si](C)(C)C(C)(C)C
null
null
C(Cl)(Cl)Cl
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
O=S(=O)(c1ccccc1)[C@@H]1CCC[C@H]2O[C@@H]12
C-[CH;D3;+0:1](-C)-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[CH3;D1;+0:1])-[C:4]
null
[]
null
null
null
null
1H NMR (CDCl3): δ 7.91 (m, 2H), 7.62 (m, 3H), 4.15 (ddd, J=10.4 Hz, 6.3 Hz, 4.4 Hz, 1H), 3.59 (d, J=2.4 Hz, 1H), 3.35 (d, J=3.5 Hz, 1H), 3.25 (dd, J=5.0 Hz, 4.3 Hz, 1H), 2.32 (m, 1H), 1.98 (m, 2H), 1.01 (d, J=7.2 Hz, 3H), 0.86 (s, 9H), 0.05 (s, 6H). 13C NMR (CDCl3): □138.3 134.0, 129.4, 128.4, 65.7, 65.3, 52.1, 49.4, 3...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.C1CC[C@H]2O[C@H]2C1
Other
C(Cl)(Cl)Cl
null
null
CC(C)[C@@H]1[C@@H](S(=O)(=O)c2ccccc2)[C@@H]2O[C@@H]2C[C@@H]1O[Si](C)(C)C(C)(C)C>C(Cl)(Cl)Cl>C[C@@H]1[C@@H](S(=O)(=O)c2ccccc2)[C@@H]2O[C@@H]2C[C@@H]1O[Si](C)(C)C(C)(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-78b524b9b1684a779811e8d7f54e7410
C[C@@H]1CC=C(S(=O)(=O)c2ccccc2)[C@H](O)C1>>C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O
[Li+].C[Si](C)(C)[N-][Si](C)(C)C.C1(=CC=CC=C1)S(=O)(=O)C=1[C@@H](C[C@@H](CC1)C)O.CCN(CC)CC.CS(=O)(=O)Cl.C1CCOC1>>C[C@@H]1[C@@H](CC=C(C=C1)SC1=CC=CC=C1)O
O=[S:6](=O)([C:5]1=[CH:13][CH2:14][C@@H:2]([CH3:1])[CH2:4][C@H:15]1[OH:16])[c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1>>[CH3:1][C@H:2]1[CH:3]=[CH:4][C:5]([S:6][c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)=[CH:13][CH2:14][C@H:15]1[OH:16]
C[C@@H]1CC=C(S(=O)(=O)c2ccccc2)[C@H](O)C1
C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O
null
null
C1=CC=CC=C1.CC(C)O
Reduction
OtherReaction
ead1c155d9aeb0039ff40f732db8600f7696952f022e16f5b513b79008524289
761a2706231bc8b83597d9327ed39c5d6cf596f163d1f8c30d951ba45f12f54b
C1=CC(Sc2ccccc2)=CCCC1
O=[S;H0;D4;+0:1](=O)(-[C;H0;D3;+0:2]1=[C:3]-[CH2;D2;+0:4]-[C@@H;D3;+0:5](-[C;D1;H3:6])-[CH2;D2;+0:7]-[C@H;D3;+0:8]-1-[O;D1;H1:9])-[c:10](:[c:11]):[c:12]>>[C;D1;H3:6]-[C@H;D3;+0:5]1-[C:13]=[CH;D2;+0:7]-[C;H0;D3;+0:2](-[S;H0;D2;+0:1]-[c:10](:[c:11]):[c:12])=[C:3]-[CH2;D2;+0:4]-[C@H;D3;+0:8]-1-[O;D1;H1:9]
92
[{"value": 92.0, "product": "C[C@@H]1[C@@H](CC=C(C=C1)SC1=CC=CC=C1)O", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
(4S)-4-Methyl-cyclohexa-1,5-dienesulfonyl)-benzene (29z). To a solution of 24z (355 mg, 1.40 mmol) and Et3N (0.19 mL, 1.40 mmol) in THF (10 mL) at 0° C. was added 0.11 mL (1.40 m-mol) of MsCl dropwise. After stirring at 0° C. for 1 h, the reaction mixture was cooled to −78° C., and freshly prepared LiHMDS (2.8 mL, 1.0 ...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Sulfone
Secondary alcohol.Monosulfide
C1=CCCCC1
C1=CCCCC=C1
C1=CCCCC=C1.c1ccccc1
Other
C1=CC=CC=C1.CC(C)O
0
1
C[C@@H]1CC=C(S(=O)(=O)c2ccccc2)[C@H](O)C1>C1=CC=CC=C1.CC(C)O>C[C@H]1C=CC(Sc2ccccc2)=CC[C@H]1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ddf938e6d3e84ba59942c28c81d2961f
CC(C)(C)[Si](C)(C)Cl.C[C@H]1C(S(=O)(=O)c2ccccc2)C=C(Sc2ccccc2)CC[C@H]1O[Si](C)(C)C>>C[C@@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)C(S(=O)(=O)c2ccccc2)=C[C@H]1O
C1(=CC=CC=C1)S(=O)(=O)C1[C@@H]([C@@H](CCC(=C1)SC1=CC=CC=C1)O[Si](C)(C)C)C.CC(C)(C)[Si](C)(C)Cl.N1C=NC=C1.C1CCOC1.CCCC[N+](CCCC)(CCCC)CCCC.[F-]>>C1(=CC=CC=C1)S(=O)(=O)C1=C[C@H]([C@@H]([C@@H]([C@H]1C)O[Si](C)(C)C(C)(C)C)C)O
Cl[Si:5]([CH3:6])([CH3:7])[C:8]([CH3:9])([CH3:10])[CH3:11].C[Si](C)(C)[O:4][C@H:3]1[C@@H:2]([CH3:1])[CH:14]([S:15](=[O:16])(=[O:17])[c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)[CH:24]=[C:25](Sc2ccccc2)[CH2:13][CH2:12]1>>[CH3:1][C@@H:2]1[C@H:3]([O:4][Si:5]([CH3:6])([CH3:7])[C:8]([CH3:9])([CH3:10])[CH3:11])[C@@H:12]([CH3...
CC(C)(C)[Si](C)(C)Cl.C[C@H]1C(S(=O)(=O)c2ccccc2)C=C(Sc2ccccc2)CC[C@H]1O[Si](C)(C)C
C[C@@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)C(S(=O)(=O)c2ccccc2)=C[C@H]1O
null
null
CN(C)C=O
C-C Coupling
OtherReaction
90dae55e1a53e4b0f3abc0387a901aea8b4624a7d95f6ab3ae19c8012917de80
81383a16bb4bb21d717e2433121f2f777f575ecc39db8d06952e063b871ee9b0
O=S(=O)(C1=CCCCC1)c1ccccc1
C-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2]1-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[C;H0;D3;+0:5](-S-c2:c:c:c:c:c:2)=[CH;D2;+0:6]-[CH;D3;+0:7](-[#16:8](=[O;D1;H0:9])(=[O;D1;H0:10])-[c:11])-[C@@H;D3;+0:12]-1-[C;D1;H3:13].Cl-[Si;H0;D4;+0:14](-[C;D1;H3:15])(-[C;D1;H3:16])-[C:17](-[C;D1;H3:18])(-[C;D1;H3:19])-[C;D1;H3:20]>>[C;D1;H3:18]-[C:1...
84
[{"value": 84.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@H]([C@@H]([C@@H]([C@H]1C)O[Si](C)(C)C(C)(C)C)C)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.0, "product": "C1(=CC=CC=C1)S(=O)(=O)C1=C[C@H]([C@@H]([C@@H]([C@H]1C)O[Si](C)(C)C(C)(C)C)C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": fal...
70
CELSIUS
20
HOUR
The mixture of diol 23 (585 mg, 2.07 mmol), TBSCl (1.0 g, 6.63 mmol), and imidazole (564 mg, 8.28 mmol) in DMF (5.0 mL) was stirred at 70° C. for 20 h under nitrogen. After being quenched by aqueous NH4Cl, the reaction mixture was extracted with diethyl ether (3×20 mL). The organic layers were washed with brine, dried ...
10.6084/m9.figshare.5104873.v1
null
Monosulfide.Silyl protective group.Silyl protective group
Secondary alcohol.TMS ether protective group
C1=CCCCCC1.c1ccccc1
C1=CCCCC1
C1=CCCCC1.c1ccccc1
HCl
CN(C)C=O
70
20
CC(C)(C)[Si](C)(C)Cl.C[C@H]1C(S(=O)(=O)c2ccccc2)C=C(Sc2ccccc2)CC[C@H]1O[Si](C)(C)C>CN(C)C=O>C[C@@H]1[C@H](O[Si](C)(C)C(C)(C)C)[C@@H](C)C(S(=O)(=O)c2ccccc2)=C[C@H]1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-93a7b084405c4ccdb8890c3c13a68a78
CO.Cc1ccc(C(=O)O)cc1[N+](=O)[O-]>>COC(=O)c1ccc(C)c([N+](=O)[O-])c1
CC1=C(C=C(C(=O)O)C=C1)[N+](=O)[O-].OS(=O)(=O)O.CO>>COC(C1=CC(=C(C=C1)C)[N+](=O)[O-])=O
[CH3:1][OH:2].O[C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH3:9])[c:10]([N+:11](=[O:12])[O-:13])[cH:14]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH3:9])[c:10]([N+:11](=[O:12])[O-:13])[cH:14]1
CO.Cc1ccc(C(=O)O)cc1[N+](=O)[O-]
COC(=O)c1ccc(C)c([N+](=O)[O-])c1
null
null
null
Protection
Esterification of Carboxylic Acids
9cecdbd189c6f9c3648521d17154d013842a5498de4e76e65efb1d842973340b
af0b8064f2e82ebe66c4c29d2391785ac1b993104265ccdc4d67ca79e36fa3c8
c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C;D1;H3:6]-[OH;D1;+0:7]>>[C;D1;H3:6]-[O;H0;D2;+0:7]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
98
[{"value": 98.0, "product": "COC(C1=CC(=C(C=C1)C)[N+](=O)[O-])=O", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
A solution of 4-methyl-3-nitrobenzoic acid (27.95 g, 154 mmol) in MeOH (550 mL) was treated with concentrated H2SO4 (10 mL, 188 mmol) and heated to reflux for 17 hours. The reaction was cooled and concentrated under reduced pressure. EtOAc (300 mL) and brine (400 mL) were added and the solution cooled to 0° C. 10N NaOH...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Methanol
Ester
null
null
c1ccccc1
HO-
null
0
null
CO.Cc1ccc(C(=O)O)cc1[N+](=O)[O-]>>COC(=O)c1ccc(C)c([N+](=O)[O-])c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-744fbc66c6004b2a8e9359399b847e98
COC(=O)c1ccc(C)c([N+](=O)[O-])c1>>COC(=O)c1ccc(C)c(N)c1
COC(C1=CC(=C(C=C1)C)[N+](=O)[O-])=O.CCOC(=O)C>>COC(C1=CC(=C(C=C1)C)N)=O
O=[N+:11]([O-])[c:10]1[c:8]([CH3:9])[cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:12]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH3:9])[c:10]([NH2:11])[cH:12]1
COC(=O)c1ccc(C)c([N+](=O)[O-])c1
COC(=O)c1ccc(C)c(N)c1
null
[Pd]
CO
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccccc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
100
[{"value": 100.0, "product": "COC(C1=CC(=C(C=C1)C)N)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
The ester from above (29.37 g, 150 mmol) was added to a 2L Parr hydrogenation flask and dissolved in anhydrous MeOH (200 mL) plus EtOAc (25 mL). The solution was then treated with 10% Pd/C (2.25 g, 50% wet) and fitted to a hydrogenator apparatus. After purging the flask 3 times with hydrogen gas, the mixture was shaken...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1
Other
[Pd].CO
null
1
COC(=O)c1ccc(C)c([N+](=O)[O-])c1>[Pd].CO>COC(=O)c1ccc(C)c(N)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5fcd73f86fce4816afc9ce92a1d244c5
Cc1ncccc1C(C)C.OO>>Cc1c(C(C)C)ccc[n+]1[O-]
OO.C(C)(C)C=1C(=NC=CC1)C>>C(C)(C)C=1C(=[N+](C=CC1)[O-])C
[CH3:1][c:2]1[c:3]([CH:4]([CH3:5])[CH3:6])[cH:7][cH:8][cH:9][n:10]1.O[OH:11]>>[CH3:1][c:2]1[c:3]([CH:4]([CH3:5])[CH3:6])[cH:7][cH:8][cH:9][n+:10]1[O-:11]
Cc1ncccc1C(C)C.OO
Cc1c(C(C)C)ccc[n+]1[O-]
null
null
CC(=O)O
Functional Group Interconversion
OtherReaction
d7f3c84fb751fef5567bc0e84a2e7c0afb271257e8dfb17aa871e038ff1a84c7
bf536f3bf8ed7b8faf08cf1c004ccd0a5e7fe59339402dd73ac837bb4a52f2ba
c1cc[nH+]cc1
O-[OH;D1;+0:1].[C;D1;H3:2]-[c:3](:[c:4]):[n;H0;D2;+0:5]:[c:6]:[c:7]>>[C;D1;H3:2]-[c:3](:[c:4]):[n+;H0;D3:5](-[O-;H0;D1:1]):[c:6]:[c:7]
94
[{"value": 94.0, "product": "C(C)(C)C=1C(=[N+](C=CC1)[O-])C", "details": "PERCENTYIELD", "is_desired": false}]
70
CELSIUS
18
HOUR
A 50% solution of hydrogen peroxide (24.89 mL) was slowly added to a solution of 3-isopropyl-2-methyl-pyridine (24.5 g, 183 mmol) (Ishiguro, et al., Yakugaku Zasshi (1958) 78:220) in HOAc (280 mL). The mixture was warmed to 70° C. and stirred for 18 h, then cooled to room temperature and concentrated in vacuo to remove...
10.6084/m9.figshare.5104873.v1
null
Peroxide
null
c1ccncc1
C1=CC=[NH+]C=C1
C1=CC=[NH+]C=C1
HO-
CC(=O)O
70
18
Cc1ncccc1C(C)C.OO>CC(=O)O>Cc1c(C(C)C)ccc[n+]1[O-]
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-efd252a864cb426b883c7fa6d1b0393d
Cc1c(C(C)C)ccc[n+]1[O-]>>CC(C)c1cccnc1CO
C(=O)(C(F)(F)F)OC(=O)C(F)(F)F.C(C)(C)C=1C(=[N+](C=CC1)[O-])C.C(=O)(C(F)(F)F)OC(=O)C(F)(F)F>>C(C)(C)C=1C(=NC=CC1)CO
[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][n+:8]([O-:11])[c:9]1[CH3:10]>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][n:8][c:9]1[CH2:10][OH:11]
Cc1c(C(C)C)ccc[n+]1[O-]
CC(C)c1cccnc1CO
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
7e561d7afee9600ed6bdb2a097e47ef139bafb1884a12ad7f91414ba01df7b33
0607ce9ac404b7f992b14bf13602ccd36eb29bd5911f2b79cc25c0bfd203a764
c1ccncc1
[CH3;D1;+0:1]-[c:2](:[c:3]):[n+;H0;D3:4](-[O-;H0;D1:5]):[c:6]:[c:7]>>[OH;D1;+0:5]-[CH2;D2;+0:1]-[c:2](:[c:3]):[n;H0;D2;+0:4]:[c:6]:[c:7]
99
[{"value": 99.0, "product": "C(C)(C)C=1C(=NC=CC1)CO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a stirred solution of 3-isopropyl-2-methyl-pyridine 1-oxide (26.05 g, 173 mmol) in CH2Cl2 (690 mL) was added dropwise TFAA (51.83 mL) over 30 min. under N2 then stirred for an additional 3 h. Caution: exothermic reaction on addition of TFAA. The mixture was concentrated in vacuo to a minimum volume. Brine (200 mL) w...
10.6084/m9.figshare.5104873.v1
null
null
Primary alcohol
C1=CC=[NH+]C=C1
c1ccncc1
c1ccncc1
null
C(Cl)Cl
null
3
Cc1c(C(C)C)ccc[n+]1[O-]>C(Cl)Cl>CC(C)c1cccnc1CO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ba0749203138458e9779665d38312ba7
CC(C)c1cccnc1CO>>CC(C)c1cccnc1C=O
C(C)(C)C=1C(=NC=CC1)CO>>C(C)(C)C=1C(=NC=CC1)C=O
[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][n:8][c:9]1[CH2:10][OH:11]>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][n:8][c:9]1[CH:10]=[O:11]
CC(C)c1cccnc1CO
CC(C)c1cccnc1C=O
null
O=[Mn]=O
C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccncc1
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[#7;a:5]:[c:6]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[#7;a:5]:[c:6]
61.7
[{"value": 61.0, "product": "C(C)(C)C=1C(=NC=CC1)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 61.7, "product": "C(C)(C)C=1C(=NC=CC1)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
To a vigorously stirred solution of (3-isopropyl-pyridin-2-yl)-methanol (26 g, 170 mmol) in CH2Cl2 (575 mL) was added MnO2 (105 g, 1.20 mol) under N2. The mixture was stirred for 18 h then filtered through a celite pad and concentrated in vacuo. Purification by column chromatography on silica gel (EtOAc/hexanes, 1:3) a...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccncc1
null
O=[Mn]=O.C(Cl)Cl
null
18
CC(C)c1cccnc1CO>O=[Mn]=O.C(Cl)Cl>CC(C)c1cccnc1C=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-02b10793e76e4128a3bfb4c79c287633
CC(C)c1cccnc1C1CC(=O)CC(c2ncccc2C(C)C)N1>>CC(C)c1cccnc1[C@@H]1CCC[C@H](c2ncccc2C(C)C)N1
C(Cl)Cl.C(C)(C)C=1C(=NC=CC1)C1NC(CC(C1)=O)C1=NC=CC=C1C(C)C.[OH-].[K+].O.NN>>C(C)(C)C=1C(=NC=CC1)[C@@H]1N[C@@H](CCC1)C1=NC=CC=C1C(C)C
O=[C:12]1[CH2:11][CH:10]([c:9]2[c:4]([CH:2]([CH3:1])[CH3:3])[cH:5][cH:6][cH:7][n:8]2)[NH:24][CH:14]([c:15]2[n:16][cH:17][cH:18][cH:19][c:20]2[CH:21]([CH3:22])[CH3:23])[CH2:13]1>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][n:8][c:9]1[C@@H:10]1[CH2:11][CH2:12][CH2:13][C@H:14]([c:15]2[n:16][cH:17][cH:18][cH:19][c:20]2[...
CC(C)c1cccnc1C1CC(=O)CC(c2ncccc2C(C)C)N1
CC(C)c1cccnc1[C@@H]1CCC[C@H](c2ncccc2C(C)C)N1
null
null
C(COCCO)O
Reduction
OtherReaction
480c86d699cecfc77c66c4f0456bd74413c6252cfa33cc10192db180010e8392
f9ba67182f94acd5fbe41487f8f71e26bccf898b8fc8091ef46f4363de5628d4
c1ccc([C@@H]2CCC[C@H](c3ccccn3)N2)nc1
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1>>[#7:4]1-[C:3]-[C:2]-[CH2;D2;+0:1]-[C:6]-[C:5]-1
99
[{"value": 99.0, "product": "C(C)(C)C=1C(=NC=CC1)[C@@H]1N[C@@H](CCC1)C1=NC=CC=C1C(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.5, "product": "C(C)(C)C=1C(=NC=CC1)[C@@H]1N[C@@H](CCC1)C1=NC=CC=C1C(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
To a solution of 3,3″-diisopropyl-2′,3′,5′,6′-tetrahydro-1′H-[2,2′;6′,2″]terpyridin-4′-one (106 mg, 0.314 mmol) in diethylene glycol (3 mL) were added KOH (352 mg, 6.29 mmol) and hydrazine monohydrate (0.61 mL, 12.6 mmol). The reaction mixture was heated to ˜100° C. for 1 h using a sand bath. After 1 h the temperature ...
10.6084/m9.figshare.5104873.v1
null
Ketone
null
C1CCNCC1
C1CCNCC1
c1ccncc1.C1CCNCC1.c1ccncc1
Other
C(COCCO)O
100
null
CC(C)c1cccnc1C1CC(=O)CC(c2ncccc2C(C)C)N1>C(COCCO)O>CC(C)c1cccnc1[C@@H]1CCC[C@H](c2ncccc2C(C)C)N1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a94744f385074e9fbe350ec4fe05f5ea
COC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=CC1=CNN(Cc2ccccc2)C1>>O=CCC1=CNN(Cc2ccccc2)C1
Cl.[Li+].CC(C)[N-]C(C)C.C(C1=CC=CC=C1)N1NC=C(C1)C=O.C(=O)([O-])[O-].[K+].[K+].CCOCCO.C(=O)=O.[Cl-].COC[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1>>C(C1=CC=CC=C1)N1NC=C(C1)CC=O
C[O:1][CH2:2][P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=[CH:3][C:4]1=[CH:5][NH:6][N:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1>>[O:1]=[CH:2][CH2:3][C:4]1=[CH:5][NH:6][N:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1
COC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=CC1=CNN(Cc2ccccc2)C1
O=CCC1=CNN(Cc2ccccc2)C1
null
null
O.C1CCOC1
Acylation
OtherReaction
09b9107a36f1ae0d38aaef1be8af826b4dbd28bb89f449aa890e5f5b01b29d66
d80bfbfdd53d8fededd98b451eddf72f4ce5a473f9fc28d89a5474331b440496
C1=CNN(Cc2ccccc2)C1
C-[O;H0;D2;+0:1]-[CH2;D2;+0:2]-[P+](-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1.O=[CH;D2;+0:3]-[C:4]1=[C:5]-[#7:6]-[#7:7]-[C:8]-1>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[CH2;D2;+0:3]-[C:4]1=[C:5]-[#7:6]-[#7:7]-[C:8]-1
51
[{"value": 51.0, "product": "C(C1=CC=CC=C1)N1NC=C(C1)CC=O", "details": "PERCENTYIELD", "is_desired": false}]
-15
CELSIUS
30
MINUTE
To a suspension of methoxymethyl-triphenyl-phosphonium chloride (2.06 g, 6.00 mmol) in dry THF (20 mL) cooled at −15° C. (ethyl glycol/dry ice) was added LDA (2.0 M in THF, 3.1 mL, 6.2 mmol) slowly. After the addition the mixture was stirred at −15° C. for 30 min, and a solution of 2-benzyl-1H-pyrazole-4-carbaldehyde (...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ether
Aldehyde
c1ccccc1.c1ccccc1.c1ccccc1
null
C1=CN[NH]C1.c1ccccc1
HO-
O.C1CCOC1
-15
0.5
COC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.O=CC1=CNN(Cc2ccccc2)C1>O.C1CCOC1>O=CCC1=CNN(Cc2ccccc2)C1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3a819352c303483fb22c31446bd2567e
Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1CCC1=CNN(Cc2ccccc2)C1>>Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1CCc1cn[nH]c1
C(C1=CC=CC=C1)N1NC=C(C1)CCN1[C@H](CCC[C@H]1C1=NC=CC=C1C)C1=NC=CC=C1C.CC(C)(C)[O-].[K+]>>CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CCC=1C=NNC1
c1ccc(C[N:26]2[NH:25][CH:24]=[C:23]([CH2:22][CH2:21][N:20]3[C@@H:8]([c:7]4[c:2]([CH3:1])[cH:3][cH:4][cH:5][n:6]4)[CH2:9][CH2:10][CH2:11][C@H:12]3[c:13]3[n:14][cH:15][cH:16][cH:17][c:18]3[CH3:19])[CH2:27]2)cc1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[C@H:8]1[CH2:9][CH2:10][CH2:11][C@@H:12]([c:13]2[n:14][cH:15][cH:16]...
Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1CCC1=CNN(Cc2ccccc2)C1
Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1CCc1cn[nH]c1
null
null
CS(=O)C.C1CCOC1
Reduction
OtherReaction
0ef0e7d2476c164dc4ef9783c9e090afca09f3d3affdb33868b053ddda3d6ef4
f31a913ab5bcf12fcacb773a895211f3d47e2ac9715e3c3c87407321eb648176
c1ccc([C@H]2CCC[C@@H](c3ccccn3)N2CCc2cn[nH]c2)nc1
[C:1]-[C:2]-[C;H0;D3;+0:3]1=[CH;D2;+0:4]-[NH;D2;+0:5]-[N;H0;D3;+0:6](-C-c2:c:c:c:c:c:2)-[CH2;D2;+0:7]-1>>[C:1]-[C:2]-[c;H0;D3;+0:3]1:[cH;D2;+0:4]:[n;H0;D2;+0:5]:[nH;D2;+0:6]:[cH;D2;+0:7]:1
64.4
[{"value": 64.0, "product": "CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CCC=1C=NNC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 64.4, "product": "CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CCC=1C=NNC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
140
CELSIUS
null
null
To a solution of (2′R,6′S)-1′-[2-(2-benzyl-1H-pyrazol-4-yl)-ethyl]-3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.130 g, 0.288 mmol) in dry DMSO (0.70 mL) and THF (12 mL) was added 4 Å molecular sieve (˜1 g) pre-heated at 140° C., and KOtBu (0.600 g, 5.35 mmol). The solution was bubbled with air (...
10.6084/m9.figshare.5104873.v1
null
Enamine.Hydrazine
null
c1ccccc1.C1=CN[NH]C1
c1cn[nH]c1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1cn[nH]c1
Other
CS(=O)C.C1CCOC1
140
null
Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1CCC1=CNN(Cc2ccccc2)C1>CS(=O)C.C1CCOC1>Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1CCc1cn[nH]c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a99bbec6227e4e2e9b0c57a1c96457cd
CC(C)(Br)Br.O=C1NC(=O)c2ccccc21>>O=C1c2ccccc2C(=O)N1CCCBr
BrC(C)(C)Br.C1(C=2C(C(N1)=O)=CC=CC2)=O.[K].CN(C)C=O>>BrCCCN1C(C2=CC=CC=C2C1=O)=O
Br[C:14]([CH3:12])([CH3:13])[Br:15].[O:1]=[C:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[C:9](=[O:10])[NH:11]1>>[O:1]=[C:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[C:9](=[O:10])[N:11]1[CH2:12][CH2:13][CH2:14][Br:15]
CC(C)(Br)Br.O=C1NC(=O)c2ccccc21
O=C1c2ccccc2C(=O)N1CCCBr
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
f611e1a25c8eecae07db6b8e7051174b409e359915352488fcf0aa865ea115f1
58ee6c221c641ad7f4c021795cad4d1767fad6c977d135f8d602f3a70dc4b197
O=C1NC(=O)c2ccccc21
Br-[C;H0;D4;+0:1](-[Br;D1;H0:2])(-[CH3;D1;+0:3])-[CH3;D1;+0:4].[O;D1;H0:5]=[C:6]1-[NH;D2;+0:7]-[C:8](=[O;D1;H0:9])-[c:10]:[c:11]-1>>[Br;D1;H0:2]-[CH2;D2;+0:1]-[CH2;D2;+0:4]-[CH2;D2;+0:3]-[N;H0;D3;+0:7]1-[C:8](=[O;D1;H0:9])-[c:10]:[c:11]-[C:6]-1=[O;D1;H0:5]
49
[{"value": 49.0, "product": "BrCCCN1C(C2=CC=CC=C2C1=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
90
CELSIUS
17
HOUR
To a solution of dibromopropane (0.61 mL, 6.0 mmol) in DMF (8 mL) was added potassium phthalimide (0.2756 g, 1.5 mmol), and was stirred at 90° C. for 17 hours. The mixture was concentrated, 1N NaOH (10 mL) was added, and extracted with CH2Cl2 (2×30 mL). The combined organic extracts were washed with water (1×15 mL), dr...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Unsubstituted dicarboximide
Primary halide.Substituted dicarboximide
c1ccc2c(c1)CNC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2
HBr
null
90
17
CC(C)(Br)Br.O=C1NC(=O)c2ccccc21>>O=C1c2ccccc2C(=O)N1CCCBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-798af5c23b554ecd94e682f9b9a291b4
Cc1cccnc1C#N.O=C1CCC(=O)N1Br>>N#Cc1ncccc1CBr
CC(C)(C#N)N=NC(C)(C)C#N.CC=1C(=NC=CC1)C#N.BrN1C(CCC1=O)=O.CC(=O)O>>BrCC=1C(=NC=CC1)C#N
[N:1]#[C:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[CH3:9].O=C1CCC(=O)N1[Br:10]>>[N:1]#[C:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[CH2:9][Br:10]
Cc1cccnc1C#N.O=C1CCC(=O)N1Br
N#Cc1ncccc1CBr
null
null
C(Cl)(Cl)(Cl)Cl
Functional Group Interconversion
Wohl-Ziegler bromination benzyl primary
45c0aca0d63a96f0092e6dded9c888827eaf6379dac179e1cefc99293896300a
08f5e7e34d3f321cce3e85421b38226d6240cca0939494ae61032d4f8405cf22
c1ccncc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5](-[C:6]#[N;D1;H0:7]):[#7;a:8]:[c:9]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5](-[C:6]#[N;D1;H0:7]):[#7;a:8]:[c:9]
21.4
[{"value": 21.0, "product": "BrCC=1C(=NC=CC1)C#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 21.4, "product": "BrCC=1C(=NC=CC1)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 3-methylpicolinonitrile (700 mg, 5.93 mmol) in CCl4 (15 mL) was added recrystallized N-bromosuccinimide (1.21 g, 6.82 mmol), followed by glacial HOAc (0.34 mL, 1.0 eq), and AIBN (97 mg, 0.60 mmol). The resultant mixture was heated to 65° C. for 3 hours, 80° C. for 2 hours, and then cooled to room tempe...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Primary halide
C1CCNC1
null
c1ccncc1
HO-
C(Cl)(Cl)(Cl)Cl
null
null
Cc1cccnc1C#N.O=C1CCC(=O)N1Br>C(Cl)(Cl)(Cl)Cl>N#Cc1ncccc1CBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-eda5f317d500415fb4a65748bc302b1f
Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1.N#Cc1cscc1CBr>>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1cscc1C#N
CC=1C(=NC=CC1)[C@@H]1N[C@@H](CCC1)C1=NC=CC=C1C.BrCC=1C(=CSC1)C#N.CCN(C(C)C)C(C)C>>CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC=1C(=CSC1)C#N
[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[C@@H:8]1[CH2:9][CH2:10][CH2:11][C@H:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1.Br[CH2:21][c:22]1[cH:23][s:24][cH:25][c:26]1[C:27]#[N:28]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18...
Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1.N#Cc1cscc1CBr
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1cscc1C#N
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(C2CCCC(c3ccccn3)N2Cc2ccsc2)nc1
Br-[CH2;D2;+0:1]-[c:2]1:[c:3]:[#16;a:4]:[c:5]:[c:6]:1.[c:7]:[#7;a:8]:[c:9](-[C@@H;D3;+0:10]1-[C:11]-[C:12]-[C:13]-[C@H;D3;+0:14](-[c:15](:[c:16]):[#7;a:17]:[c:18])-[NH;D2;+0:19]-1):[c:20]>>[c:7]:[#7;a:8]:[c:9](-[CH;D3;+0:10]1-[C:11]-[C:12]-[C:13]-[CH;D3;+0:14](-[c:15](:[c:16]):[#7;a:17]:[c:18])-[N;H0;D3;+0:19]-1-[CH2;D...
84
[{"value": 84.0, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC=1C(=CSC1)C#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.1, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC=1C(=CSC1)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: A solution of 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-cis-[2,2′;6′,2″]terpyridine (0.097 g, 0.37 mmol), 4-bromomethyl-thiophene-3-carbonitrile (0.168 g, 0.83 mmol) (Terpstra, J. W., et al., J. Org. Chem. (1986) 51:230-238), KI (21 mg, 0.13 mmol), and DIPEA (0.15 mL, 0.86 mmol) in DMF (3 mL)...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccsc1
HBr
CN(C)C=O
null
null
Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1.N#Cc1cscc1CBr>CN(C)C=O>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1cscc1C#N
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-53ada5f6a5134fde91e72f7c8481bc5d
CS(=O)(=O)Cl.OCCc1cncs1>>CS(=O)(=O)OCCc1cncs1
O.S1C=NC=C1CCO.CS(=O)(=O)Cl.CCN(CC)CC>>S1C=NC=C1CCOS(=O)(=O)C
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][CH2:7][c:8]1[cH:9][n:10][cH:11][s:12]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][CH2:7][c:8]1[cH:9][n:10][cH:11][s:12]1
CS(=O)(=O)Cl.OCCc1cncs1
CS(=O)(=O)OCCc1cncs1
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1cscn1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6]-[OH;D1;+0:7]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
100
[{"value": 100.0, "product": "S1C=NC=C1CCOS(=O)(=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.7, "product": "S1C=NC=C1CCOS(=O)(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
At 0° C., to a solution of 2-thiazol-5-yl-ethanol (0.154 g, 1.19 mmol) in CH2Cl2 (10 mL) was added MsCl (0.150 g, 1.31 mmol) and Et3N (0.180 g, 1.79 mmol). The mixture was stirred at room temperature for 1 h. Water (20 mL) was added, and the mixture was extracted with CH2Cl2 (3×30 mL). The extracts were combined and dr...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1cscn1
HCl
C(Cl)Cl
null
1
CS(=O)(=O)Cl.OCCc1cncs1>C(Cl)Cl>CS(=O)(=O)OCCc1cncs1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e49c06edb6844f65a15f673b085d9f81
CS(=O)(=O)Cl.O=[N+]([O-])c1ccccc1S(=O)(=O)N(Cc1ccc(CO)cc1)Cc1ccccn1>>CS(=O)(=O)OCc1ccc(CN(Cc2ccccn2)S(=O)(=O)c2ccccc2[N+](=O)[O-])cc1
C(=O)(O)[O-].[Na+].OCC1=CC=C(CN(S(=O)(=O)C2=C(C=CC=C2)[N+](=O)[O-])CC2=NC=CC=C2)C=C1.CCN(CC)CC.CS(=O)(=O)Cl.CCN(CC)CC.CS(=O)(=O)Cl>>[N+](=O)([O-])C1=C(C=CC=C1)S(=O)(=O)N(CC1=NC=CC=C1)CC1=CC=C(COS(=O)(=O)C)C=C1
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][c:7]1[cH:8][cH:9][c:10]([CH2:11][N:12]([CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][n:19]2)[S:20](=[O:21])(=[O:22])[c:23]2[cH:24][cH:25][cH:26][cH:27][c:28]2[N+:29](=[O:30])[O-:31])[cH:32][cH:33]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][c:7]1[cH:8][cH:9][c:10]([CH2:11][N:12...
CS(=O)(=O)Cl.O=[N+]([O-])c1ccccc1S(=O)(=O)N(Cc1ccc(CO)cc1)Cc1ccccn1
CS(=O)(=O)OCc1ccc(CN(Cc2ccccn2)S(=O)(=O)c2ccccc2[N+](=O)[O-])cc1
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
O=S(=O)(c1ccccc1)N(Cc1ccccc1)Cc1ccccn1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[OH;D1;+0:5]-[C:6]-[c:7]>>[C;D1;H3:2]-[S;H0;D4;+0:1](=[O;D1;H0:3])(=[O;D1;H0:4])-[O;H0;D2;+0:5]-[C:6]-[c:7]
95
[{"value": 95.0, "product": "[N+](=O)([O-])C1=C(C=CC=C1)S(=O)(=O)N(CC1=NC=CC=C1)CC1=CC=C(COS(=O)(=O)C)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
To a stirring solution of N-(4-hydroxymethyl-benzyl)-2-nitro-N-pyridin-2-ylmethyl-benzenesulfonamide (Bridger, et al., U.S. Ser. No. 09/111,895) (0.2096 g, 0.51 mmol) in CH2Cl2 (5 mL) at 0° C. under Ar, was added Et3N (0.14 mL, 1.02 mmol) and MsCl (0.05 mL, 0.66 mmol). The mixture was stirred at 0° C. for 2 hours, then...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1ccccc1.c1ccncc1.c1ccccc1
HCl
C(Cl)Cl
0
2
CS(=O)(=O)Cl.O=[N+]([O-])c1ccccc1S(=O)(=O)N(Cc1ccc(CO)cc1)Cc1ccccn1>C(Cl)Cl>CS(=O)(=O)OCc1ccc(CN(Cc2ccccn2)S(=O)(=O)c2ccccc2[N+](=O)[O-])cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-384691ba1af0445eb367e3e072844f60
Cc1cnc(CO)c(C)c1>>Cc1cnc(C=O)c(C)c1
CC=1C(=NC=C(C1)C)CO>>CC=1C(=NC=C(C1)C)C=O
[CH3:1][c:2]1[cH:3][n:4][c:5]([CH2:6][OH:7])[c:8]([CH3:9])[cH:10]1>>[CH3:1][c:2]1[cH:3][n:4][c:5]([CH:6]=[O:7])[c:8]([CH3:9])[cH:10]1
Cc1cnc(CO)c(C)c1
Cc1cnc(C=O)c(C)c1
null
O=[Mn]=O
C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccncc1
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[#7;a:5]:[c:6]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[#7;a:5]:[c:6]
null
[]
null
null
null
null
To a solution of (3,5-dimethyl-pyridin-2-yl)-methanol (2.12 g, 15.45 mmol) (Weidmann, K., et al., J. Med. Chem. (1992) 35:438-450) in CH2Cl2 (50 mL) was added MnO2 (9.41 g, 108.18 mmol) and the reaction mixture was refluxed overnight. Then it was cooled and the mixture was filtered through a layer of celite. The filtra...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccncc1
null
O=[Mn]=O.C(Cl)Cl
null
null
Cc1cnc(CO)c(C)c1>O=[Mn]=O.C(Cl)Cl>Cc1cnc(C=O)c(C)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3f169f4154fd4ae78f611376589451ea
Cc1cccnc1C1CC(C)(O)CC(c2ncccc2C)N1.O=C1c2ccccc2C(=O)N1CCCCBr>>Cc1cccnc1C1CC(C)(O)CC(c2ncccc2C)N1CCCCN1C(=O)c2ccccc2C1=O
CC=1C(=NC=CC1)C1NC(CC(C1)(O)C)C1=NC=CC=C1C.BrCCCCN1C(C2=CC=CC=C2C1=O)=O.CCN(C(C)C)C(C)C>>OC1(CC(N(C(C1)C1=NC=CC=C1C)CCCCN1C(C2=CC=CC=C2C1=O)=O)C1=NC=CC=C1C)C
[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][C:10]([CH3:11])([OH:12])[CH2:13][CH:14]([c:15]2[n:16][cH:17][cH:18][cH:19][c:20]2[CH3:21])[NH:22]1.Br[CH2:23][CH2:24][CH2:25][CH2:26][N:27]1[C:28](=[O:29])[c:30]2[cH:31][cH:32][cH:33][cH:34][c:35]2[C:36]1=[O:37]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[...
Cc1cccnc1C1CC(C)(O)CC(c2ncccc2C)N1.O=C1c2ccccc2C(=O)N1CCCCBr
Cc1cccnc1C1CC(C)(O)CC(c2ncccc2C)N1CCCCN1C(=O)c2ccccc2C1=O
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1c2ccccc2C(=O)N1CCCCN1C(c2ccccn2)CCCC1c1ccccn1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7;a:4]:[c:5]-[C:6](-[C:7])-[NH;D2;+0:8]-[C:9](-[c:10]:[#7;a:11])-[C:12]>>[#7;a:4]:[c:5]-[C:6](-[C:7])-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3])-[C:9](-[c:10]:[#7;a:11])-[C:12]
null
[]
60
CELSIUS
24
HOUR
To a solution of meso-2′β,6′β-[3,4′,3″-trimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridin-4′-ol (0.2499 g, 0.84 mmol) in DMF (9 mL) was added 2-(4-bromo-butyl)-isoindole-1,3-dione (0.2605 g, 0.92 mmol), KI (0.0142 g, 0.08 mmol), and DIPEA (0.29 mL, 1.68 mmol), and stirred at 60° C. for 24 hours. The mixture w...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccc2c(c1)C[NH]C2
HBr
CN(C)C=O
60
24
Cc1cccnc1C1CC(C)(O)CC(c2ncccc2C)N1.O=C1c2ccccc2C(=O)N1CCCCBr>CN(C)C=O>Cc1cccnc1C1CC(C)(O)CC(c2ncccc2C)N1CCCCN1C(=O)c2ccccc2C1=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-551da803035448cea5dce0c49a883354
COC(=O)c1cc(C#N)ccc1CBr.Cc1cccnc1C1CCCC(c2ncccc2C)N1>>COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.COC(C1=C(C=CC(=C1)C#N)CBr)=O>>COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)=O
Br[CH2:13][c:12]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:6][c:7]([C:8]#[N:9])[cH:10][cH:11]1.[NH:14]1[CH:15]([c:16]2[n:17][cH:18][cH:19][cH:20][c:21]2[CH3:22])[CH2:23][CH2:24][CH2:25][CH:26]1[c:27]1[n:28][cH:29][cH:30][cH:31][c:32]1[CH3:33]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([C:8]#[N:9])[cH:10][cH:11][c:12]1[CH2:1...
COC(=O)c1cc(C#N)ccc1CBr.Cc1cccnc1C1CCCC(c2ncccc2C)N1
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7].[#7;a:8]:[c:9]-[C:10](-[C:11])-[NH;D2;+0:12]-[C:13](-[c:14]:[#7;a:15])-[C:16]>>[#7;a:8]:[c:9]-[C:10](-[C:11])-[N;H0;D3;+0:12](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7])-[C:13](-[c:14]:[#7;a:15])-[C:16]
78
[{"value": 78.0, "product": "COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.6, "product": "COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Following General Procedure A: 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (1.6 g, 6.0 mmol) was reacted with 2-bromomethyl-5-cyano-benzoic acid methyl ester (1.5 g, 6.0 mmol) to give 5-cyano-2-(3,3″-dimethyl-3′,4′,5′,6′-tetrahydro-2′H-[2,2′;6′,2″]terpyridin-1′-ylmethyl)-benzoic acid methyl ester ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccccc1.c1ccncc1.C1CC[NH]CC1.c1ccncc1
HBr
null
null
null
COC(=O)c1cc(C#N)ccc1CBr.Cc1cccnc1C1CCCC(c2ncccc2C)N1>>COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a9159759d5ba40b1905a655940fbe6f2
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C>>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1CO
COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)=O.[Li+].[BH4-]>>CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C=C(C#N)C=C1)CO
CO[C:30]([c:29]1[c:22]([CH2:21][N:20]2[CH:8]([c:7]3[c:2]([CH3:1])[cH:3][cH:4][cH:5][n:6]3)[CH2:9][CH2:10][CH2:11][CH:12]2[c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[cH:23][cH:24][c:25]([C:26]#[N:27])[cH:28]1)=[O:31]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH...
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1CO
null
null
CO
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3](:[c:4]):[c:5]>>[OH;D1;+0:2]-[CH2;D2;+0:1]-[c:3](:[c:4]):[c:5]
86
[{"value": 86.0, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C=C(C#N)C=C1)CO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3.5
HOUR
To a stirred, room temperature solution of the ester from above (2.05 g, 4.6 mmol) in MeOH (50 mL) was added LiBH4 (1.0 g, 50 mmol) in three portions. Effervescence was observed, and the mixture was stirred for 3.5 hours. The mixture was concentrated and 1 N NaOH (50 mL) was added to the resultant residue. The aqueous ...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1
Other
CO
null
3.5
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C>CO>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1CO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-1e472432ad8f4a5b837c819eb7a792f7
Cc1ccc(Br)c(F)c1>>Cc1ccc(C#N)c(F)c1
BrC1=C(C=C(C=C1)C)F.CN(C)C=O>>FC1=C(C#N)C=CC(=C1)C
Br[c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:10][c:8]1[F:9]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([C:6]#[N:7])[c:8]([F:9])[cH:10]1
Cc1ccc(Br)c(F)c1
Cc1ccc(C#N)c(F)c1
null
[C-]#N.[C-]#N.[Zn+2].C1(=CC=CC=C1)P([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2].C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd]
null
Miscellaneous
OtherReaction
3ae4da8b7f110de99cf8afc091b6f0c8540050148e425770f8030bce1480042c
73a96fe5e833259ca394a42f82d6cc2ee7231bcde92d95030d2893b90c3fef76
c1ccccc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[F;D1;H0:5]):[c:6]>>[F;D1;H0:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[C:7]#[N;D1;H0:8]):[c:2]:[c:3]
65
[{"value": 65.0, "product": "FC1=C(C#N)C=CC(=C1)C", "details": "PERCENTYIELD", "is_desired": false}]
130
CELSIUS
null
null
Under N2, to a suspension of 1-bromo-2-fluoro-4-methyl-benzene (2.59 g, 13.7 mmol) and Zn(CN)2 (1.60 g, 13.7 mmol) in dry DMF (50 mL) was added 1,1′-bis(diphenylphosphino)ferrocene (DPPF) (0.0753 g, 0.136 mmol) and Pd2(dba)3 (dba=di(benzylidene)acetone) (0.0623 g, 0.0681 mmol). After the mixture was heated at 130° C. f...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Nitrile
c1ccccc1
c1ccccc1
c1ccccc1
Br-
[C-]#N.[C-]#N.[Zn+2].C1(=CC=CC=C1)P([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2].C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd]
130
null
Cc1ccc(Br)c(F)c1>[C-]#N.[C-]#N.[Zn+2].C1(=CC=CC=C1)P([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2].C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd]>Cc1ccc(C#N)c(F)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9895fd7b8454479c8a6517c73ce07583
Cc1ccc(C#N)c(F)c1.O=C1CCC(=O)N1Br>>N#Cc1ccc(CBr)cc1F
[O-]S(=O)(=S)[O-].[Na+].[Na+].FC1=C(C#N)C=CC(=C1)C.N(=NC1(CCCCC1)C#N)C1(CCCCC1)C#N.C1CC(=O)N(C1=O)Br>>BrCC1=CC(=C(C#N)C=C1)F
[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([CH3:7])[cH:9][c:10]1[F:11].O=C1CCC(=O)N1[Br:8]>>[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][Br:8])[cH:9][c:10]1[F:11]
Cc1ccc(C#N)c(F)c1.O=C1CCC(=O)N1Br
N#Cc1ccc(CBr)cc1F
null
null
O.C(Cl)(Cl)(Cl)Cl
Functional Group Interconversion
Wohl-Ziegler bromination benzyl primary
45c0aca0d63a96f0092e6dded9c888827eaf6379dac179e1cefc99293896300a
08f5e7e34d3f321cce3e85421b38226d6240cca0939494ae61032d4f8405cf22
c1ccccc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]
65.1
[{"value": 65.0, "product": "BrCC1=CC(=C(C#N)C=C1)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 65.1, "product": "BrCC1=CC(=C(C#N)C=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 2-fluoro-4-methyl-benzonitrile (1.45 g, 10.7 mmol) in CCl4 (100 mL) was added 1,1′-azobis(cyclohexanecarbonitrile) (0.240 g, 0.982 mmol) and NBS (2.19 g, 12.3 mmol). The mixture was stirred and heated at reflux overnight, and then cooled to room temperature. A solution of Na2S2O3 (5 g) in H2O (100 mL) ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Primary halide
C1CCNC1
null
c1ccccc1
HO-
O.C(Cl)(Cl)(Cl)Cl
null
null
Cc1ccc(C#N)c(F)c1.O=C1CCC(=O)N1Br>O.C(Cl)(Cl)(Cl)Cl>N#Cc1ccc(CBr)cc1F
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b7b50d1e207e4d1fad21507dc139f2b0
Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1.N#Cc1ccc(CBr)cc1F>>Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc(C#N)c(F)c1
CC=1C(=NC=CC1)[C@@H]1N[C@@H](CCC1)C1=NC=CC=C1C.BrCC1=CC(=C(C#N)C=C1)F.CCN(C(C)C)C(C)C>>CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CC1=CC(=C(C#N)C=C1)F
[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[C@@H:8]1[CH2:9][CH2:10][CH2:11][C@H:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1.Br[CH2:21][c:22]1[cH:23][cH:24][c:25]([C:26]#[N:27])[c:28]([F:29])[cH:30]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[C@H:8]1[CH2:9][CH2:10][CH2:11][C@@H:12]([c:13]2[n:14][cH:15...
Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1.N#Cc1ccc(CBr)cc1F
Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc(C#N)c(F)c1
null
null
CC#N
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2[C@@H](c3ccccn3)CCC[C@H]2c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[#7;a:5]:[c:6]-[C:7](-[C:8])-[NH;D2;+0:9]-[C:10](-[c:11]:[#7;a:12])-[C:13]>>[#7;a:5]:[c:6]-[C:7](-[C:8])-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10](-[c:11]:[#7;a:12])-[C:13]
100
[{"value": 100.0, "product": "CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CC1=CC(=C(C#N)C=C1)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.9, "product": "CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CC1=CC(=C(C#N)C=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
16
HOUR
A mixture of (2′R,6′S)-3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.267 g, 1.00 mmol), 4-bromomethyl-2-fluoro-benzonitrile (0.321 g, 0.1.50 mmol), DIPEA (0.259 g, 2.00 mmol) and KI (0.017 g, 0.10 mmol) in dry CH3CN (10 mL) was stirred at 60° C. for 16 h. After that period of time the CH3CN was r...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1
HBr
CC#N
60
16
Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1.N#Cc1ccc(CBr)cc1F>CC#N>Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc(C#N)c(F)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-41ffeaac47594f33aa948715cc781f89
CC(C)=NO.Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc(C#N)c(F)c1>>CC(C)=NOc1cc(CN2[C@@H](c3ncccc3C)CCC[C@H]2c2ncccc2C)ccc1C#N
CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CC1=CC(=C(C#N)C=C1)F.CC(C)([O-])C.[K+].CC(C)=NO>>CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CC1=CC(=C(C#N)C=C1)ON=C(C)C
[CH3:1][C:2]([CH3:3])=[N:4][OH:5].F[c:6]1[cH:7][c:8]([CH2:9][N:10]2[C@@H:11]([c:12]3[n:13][cH:14][cH:15][cH:16][c:17]3[CH3:18])[CH2:19][CH2:20][CH2:21][C@H:22]2[c:23]2[n:24][cH:25][cH:26][cH:27][c:28]2[CH3:29])[cH:30][cH:31][c:32]1[C:33]#[N:34]>>[CH3:1][C:2]([CH3:3])=[N:4][O:5][c:6]1[cH:7][c:8]([CH2:9][N:10]2[C@@H:11](...
CC(C)=NO.Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc(C#N)c(F)c1
CC(C)=NOc1cc(CN2[C@@H](c3ncccc3C)CCC[C@H]2c2ncccc2C)ccc1C#N
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
4074777e8d881b991351d02d1bc762626b9bc33d60e315f16350fd17e7674c5e
16e2061367461bda1ff490f3d967aaccaa7d481e8df8d02752e2a63e0ea13301
c1ccc(CN2[C@@H](c3ccccn3)CCC[C@H]2c2ccccn2)cc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[C;D1;H3:8]-[C:9](-[C;D1;H3:10])=[#7:11]-[OH;D1;+0:12]>>[C;D1;H3:8]-[C:9](-[C;D1;H3:10])=[#7:11]-[O;H0;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7]
69
[{"value": 69.0, "product": "CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CC1=CC(=C(C#N)C=C1)ON=C(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 68.6, "product": "CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CC1=CC(=C(C#N)C=C1)ON=C(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of potassium tert-butoxide (0.140 g, 1.25 mmol) in dry DMF (5 mL) was added acetone oxime (0.0877 g, 1.20 mmol), and the mixture was stirred for 30 min. A solution of 4-((2′R,6′S)-3,3″-dimethyl-3′,4′,5′,6′-tetrahydro-2′H-[2,2′;6′,2″]terpyridin-1′-ylmethyl)-2-fluoro-benzonitrile (0.400 g, 1.00 mmol) in dry...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Oxime
null
c1ccccc1
c1ccccc1
c1ccccc1.c1ccncc1.C1CC[NH]CC1.c1ccncc1
HF
CN(C)C=O
null
0.5
CC(C)=NO.Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc(C#N)c(F)c1>CN(C)C=O>CC(C)=NOc1cc(CN2[C@@H](c3ncccc3C)CCC[C@H]2c2ncccc2C)ccc1C#N
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-64e1b511083d4b89a70af233551c73c8
CC(C)=NOc1cc(CN2[C@@H](c3ncccc3C)CCC[C@H]2c2ncccc2C)ccc1C#N>>Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc2c(N)noc2c1
CC=1C(=NC=CC1)[C@@H]1N([C@@H](CCC1)C1=NC=CC=C1C)CC1=CC(=C(C#N)C=C1)ON=C(C)C.Cl>>CC=1C(=NC=CC1)[C@H]1N([C@H](CCC1)C1=NC=CC=C1C)CC1=CC2=C(C(=NO2)N)C=C1
CC(C)=[N:28][O:29][c:30]1[c:25]([C:26]#[N:27])[cH:24][cH:23][c:22]([CH2:21][N:20]2[C@H:8]([c:7]3[c:2]([CH3:1])[cH:3][cH:4][cH:5][n:6]3)[CH2:9][CH2:10][CH2:11][C@@H:12]2[c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[cH:31]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[C@H:8]1[CH2:9][CH2:10][CH2:11][C@@H:12]([c:13]2[n...
CC(C)=NOc1cc(CN2[C@@H](c3ncccc3C)CCC[C@H]2c2ncccc2C)ccc1C#N
Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc2c(N)noc2c1
null
null
CCO
Aromatic Heterocycle Formation
OtherReaction
b0c8b6cab702ae896823dfc39bf3c91df5af1f06a524f3e4589ddf87232b1bc2
f7bbda299ac8fe6ebc980c7e96a23faca5969207a0ba4ec41cb02caa3616b51d
c1ccc([C@H]2CCC[C@@H](c3ccccn3)N2Cc2ccc3cnoc3c2)nc1
C-C(-C)=[N;H0;D2;+0:1]-[O;H0;D2;+0:2]-[c:3](:[c:4]):[c:5](-[C;H0;D2;+0:6]#[N;H0;D1;+0:7]):[c:8]>>[NH2;D1;+0:7]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:1]:[o;H0;D2;+0:2]:[c:3](:[c:4]):[c:5]:1:[c:8]
62
[{"value": 62.0, "product": "CC=1C(=NC=CC1)[C@H]1N([C@H](CCC1)C1=NC=CC=C1C)CC1=CC2=C(C(=NO2)N)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.0, "product": "CC=1C(=NC=CC1)[C@H]1N([C@H](CCC1)C1=NC=CC=C1C)CC1=CC2=C(C(=NO2)N)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 4-((2′R,6′S)-3,3″-dimethyl-3′,4′,5′,6′-tetrahydro-2′H-[2,2′;6′,2″]terpyridin-1′-ylmethyl)-2-isopropylideneaminooxy-benzonitrile (0.145 g, 0.320 mmol) in EtOH (4 mL) was added aqueous HCl (3 N, 4 mL), and the mixture was stirred and heated at reflux overnight. The mixture was then cooled to room tempera...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
c1ccccc1
c1ccc2oncc2c1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccc2oncc2c1
Other
CCO
null
null
CC(C)=NOc1cc(CN2[C@@H](c3ncccc3C)CCC[C@H]2c2ncccc2C)ccc1C#N>CCO>Cc1cccnc1[C@H]1CCC[C@@H](c2ncccc2C)N1Cc1ccc2c(N)noc2c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e89c238f80f842dc9a596346db785b73
COC(=O)c1cc(C#N)ccc1C.O=S(=O)(O)O>>Cc1ccc(C(=O)O)cc1C(=O)O
COC(C1=C(C=CC(=C1)C#N)C)=O.S(O)(O)(=O)=O.O>>CC1=C(C=C(C(=O)O)C=C1)C(=O)O
C[O:13][C:11]([c:10]1[c:2]([CH3:1])[cH:3][cH:4][c:5]([C:6]#N)[cH:9]1)=[O:12].O=S(=O)([OH:7])[OH:8]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([C:6](=[O:7])[OH:8])[cH:9][c:10]1[C:11](=[O:12])[OH:13]
COC(=O)c1cc(C#N)ccc1C.O=S(=O)(O)O
Cc1ccc(C(=O)O)cc1C(=O)O
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
04f6f47359a38696a2f676a2c8a4c8f2bdd2e4c4c96cb5a4094b7353433a7559
a005c00caf42b66f67212cff26e6319025c9c1a53adbd7d3253c8ef6782e7b51
c1ccccc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4]:[c:5]:[c:6](-[C;H0;D2;+0:7]#N):[c:8].O=S(=O)(-[OH;D1;+0:9])-[OH;D1;+0:10]>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4]:[c:5]:[c:6](-[C;H0;D3;+0:7](=[O;H0;D1;+0:9])-[OH;D1;+0:10]):[c:8]
null
[]
150
CELSIUS
4
HOUR
5-Cyano-2-methyl-benzoic acid methyl ester (1.09 g, 6.22 mmol) was suspended in a mixture of water (25 mL) and concentrated sulfuric acid (10 mL). The yellow solution was stirred at 150° C. for 4 hours to give a pale yellow slurry. The reaction mixture was cooled to room temperature and the precipitate was isolated via...
10.6084/m9.figshare.5104873.v1
null
Ester.Nitrile
Carboxylic acid.Carboxylic acid
null
null
c1ccccc1
HO-
null
150
4
COC(=O)c1cc(C#N)ccc1C.O=S(=O)(O)O>>Cc1ccc(C(=O)O)cc1C(=O)O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-da4dcd5cf6f748469c422da922640649
COC(=O)c1ccc(C)c(C(=O)OC)c1.O=C1CCC(=O)N1Br>>COC(=O)c1ccc(CBr)c(C(=O)OC)c1
N(=NC1(CCCCC1)C#N)C1(CCCCC1)C#N.COC(C1=CC(C(=O)OC)=C(C=C1)C)=O.BrN1C(CCC1=O)=O>>COC(C1=CC(C(=O)OC)=C(C=C1)CBr)=O
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH3:9])[c:11]([C:12](=[O:13])[O:14][CH3:15])[cH:16]1.O=C1CCC(=O)N1[Br:10]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH2:9][Br:10])[c:11]([C:12](=[O:13])[O:14][CH3:15])[cH:16]1
COC(=O)c1ccc(C)c(C(=O)OC)c1.O=C1CCC(=O)N1Br
COC(=O)c1ccc(CBr)c(C(=O)OC)c1
null
null
C(Cl)(Cl)(Cl)Cl
Functional Group Interconversion
Wohl-Ziegler bromination benzyl primary
45c0aca0d63a96f0092e6dded9c888827eaf6379dac179e1cefc99293896300a
08f5e7e34d3f321cce3e85421b38226d6240cca0939494ae61032d4f8405cf22
c1ccccc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[#8:2]-[C:3](=[O;D1;H0:4])-[c:5]:[c:6](-[CH3;D1;+0:7]):[c:8]>>[#8:2]-[C:3](=[O;D1;H0:4])-[c:5]:[c:6](-[CH2;D2;+0:7]-[Br;H0;D1;+0:1]):[c:8]
72
[{"value": 72.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Methyl-isophthalic acid dimethyl ester (1.06 g, 5.10 mmol), N-bromosuccinimide (1.00 g, 5.61 mmol) and 1,1′-azobis(cyclohexanecarbonitrile) (0.31 g, 1.27 mmol) were suspended in carbon tetrachloride (22 mL) and the resulting mixture was refluxed for 16 hours under N2. The orange solution was concentrated under reduce...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Primary halide
C1CCNC1
null
c1ccccc1
HO-
C(Cl)(Cl)(Cl)Cl
null
null
COC(=O)c1ccc(C)c(C(=O)OC)c1.O=C1CCC(=O)N1Br>C(Cl)(Cl)(Cl)Cl>COC(=O)c1ccc(CBr)c(C(=O)OC)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-cd83c06abdbc466b91d443a6d698ad5a
COC(=O)c1cc(C#N)ccc1CBr.Cc1cccnc1C1CCCC(c2ncccc2C)N1>>COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.COC(C1=C(C=CC(=C1)C#N)CBr)=O.CCN(C(C)C)C(C)C>>COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)=O
Br[CH2:13][c:12]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:6][c:7]([C:8]#[N:9])[cH:10][cH:11]1.[NH:14]1[CH:15]([c:16]2[n:17][cH:18][cH:19][cH:20][c:21]2[CH3:22])[CH2:23][CH2:24][CH2:25][CH:26]1[c:27]1[n:28][cH:29][cH:30][cH:31][c:32]1[CH3:33]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([C:8]#[N:9])[cH:10][cH:11][c:12]1[CH2:1...
COC(=O)c1cc(C#N)ccc1CBr.Cc1cccnc1C1CCCC(c2ncccc2C)N1
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7].[#7;a:8]:[c:9]-[C:10](-[C:11])-[NH;D2;+0:12]-[C:13](-[c:14]:[#7;a:15])-[C:16]>>[#7;a:8]:[c:9]-[C:10](-[C:11])-[N;H0;D3;+0:12](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7])-[C:13](-[c:14]:[#7;a:15])-[C:16]
96.1
[{"value": 96.0, "product": "COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.1, "product": "COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: A solution of 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.260 g, 0.98 mmol), 2-bromomethyl-5-cyano-benzoic acid methyl ester (0.360 g, 1.42 mmol), KI (37 mg, 0.22 mmol), and DIPEA (0.35 mL, 2.01 mmol) in DMF (5 mL) was heated at 60° C. for 17 hours. Purification of th...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccccc1.c1ccncc1.C1CC[NH]CC1.c1ccncc1
HBr
CN(C)C=O
null
null
COC(=O)c1cc(C#N)ccc1CBr.Cc1cccnc1C1CCCC(c2ncccc2C)N1>CN(C)C=O>COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2C)CCCC1c1ncccc1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-72f2007f948d4e52b9d8b0a1553167a4
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1ccccc1CBr>>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccccc1C#N
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.BrCC=1C(=CC=CC1)C#N.CCN(C(C)C)C(C)C>>CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C#N)C=CC=C1
[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1.Br[CH2:21][c:22]1[cH:23][cH:24][cH:25][cH:26][c:27]1[C:28]#[N:29]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17]...
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1ccccc1CBr
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccccc1C#N
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[#7;a:5]:[c:6]-[C:7](-[C:8])-[NH;D2;+0:9]-[C:10](-[c:11]:[#7;a:12])-[C:13]>>[#7;a:5]:[c:6]-[C:7](-[C:8])-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10](-[c:11]:[#7;a:12])-[C:13]
91
[{"value": 91.0, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C#N)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.6, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C#N)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: A solution of 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.602 g, 2.25 mmol), α-bromo-o-tolunitrile (0.668 g, 3.41 mmol), KI (100 mg, 0.60 mmol), and DIPEA (0.80 mL, 4.59 mmol) in DMF (11 mL) was heated at 60° C. for 23 hours. Purification of the crude material by colu...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1
HBr
CN(C)C=O
null
null
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1ccccc1CBr>CN(C)C=O>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccccc1C#N
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-99bd945b17484da2b882e142999adcdf
CO.Cc1ccc(C(=O)O)cc1[N+](=O)[O-]>>COC(=O)c1ccc(C)c([N+](=O)[O-])c1
CC1=C(C=C(C(=O)O)C=C1)[N+](=O)[O-].S(O)(O)(=O)=O.CO>>COC(C1=CC(=C(C=C1)C)[N+](=O)[O-])=O
[CH3:1][OH:2].O[C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH3:9])[c:10]([N+:11](=[O:12])[O-:13])[cH:14]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH3:9])[c:10]([N+:11](=[O:12])[O-:13])[cH:14]1
CO.Cc1ccc(C(=O)O)cc1[N+](=O)[O-]
COC(=O)c1ccc(C)c([N+](=O)[O-])c1
null
null
null
Protection
Esterification of Carboxylic Acids
9cecdbd189c6f9c3648521d17154d013842a5498de4e76e65efb1d842973340b
af0b8064f2e82ebe66c4c29d2391785ac1b993104265ccdc4d67ca79e36fa3c8
c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C;D1;H3:6]-[OH;D1;+0:7]>>[C;D1;H3:6]-[O;H0;D2;+0:7]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
97
[{"value": 97.0, "product": "COC(C1=CC(=C(C=C1)C)[N+](=O)[O-])=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 4-methyl-3-nitrobenzoic acid (5.52 g, 30.5 mmol) in MeOH (100 mL) was added 98% sulfuric acid (2 mL) and the resultant mixture was refluxed overnight, then cooled to room temperature. The mixture was concentrated and the residue was dissolved in CH2Cl2 (50 mL) and water (20 mL). Solid Na2CO3 was added ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Methanol
Ester
null
null
c1ccccc1
HO-
null
null
null
CO.Cc1ccc(C(=O)O)cc1[N+](=O)[O-]>>COC(=O)c1ccc(C)c([N+](=O)[O-])c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-4d5cc9c759a04a9da593bc4c28b37f28
COC(=O)c1ccc(C)c([N+](=O)[O-])c1.O=C1CCC(=O)N1Br>>COC(=O)c1ccc(CBr)c([N+](=O)[O-])c1
N(=NC1(CCCCC1)C#N)C1(CCCCC1)C#N.COC(C1=CC(=C(C=C1)C)[N+](=O)[O-])=O.BrN1C(CCC1=O)=O>>COC(C1=CC(=C(C=C1)CBr)[N+](=O)[O-])=O
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH3:9])[c:11]([N+:12](=[O:13])[O-:14])[cH:15]1.O=C1CCC(=O)N1[Br:10]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH2:9][Br:10])[c:11]([N+:12](=[O:13])[O-:14])[cH:15]1
COC(=O)c1ccc(C)c([N+](=O)[O-])c1.O=C1CCC(=O)N1Br
COC(=O)c1ccc(CBr)c([N+](=O)[O-])c1
null
null
C(Cl)(Cl)(Cl)Cl
Functional Group Interconversion
Wohl-Ziegler bromination benzyl primary
45c0aca0d63a96f0092e6dded9c888827eaf6379dac179e1cefc99293896300a
08f5e7e34d3f321cce3e85421b38226d6240cca0939494ae61032d4f8405cf22
c1ccccc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]
61
[{"value": 61.0, "product": "COC(C1=CC(=C(C=C1)CBr)[N+](=O)[O-])=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 61.0, "product": "COC(C1=CC(=C(C=C1)CBr)[N+](=O)[O-])=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 4-methyl-3-nitrobenzoic acid (5.52 g, 30.5 mmol) in MeOH (100 mL) was added 98% sulfuric acid (2 mL) and the resultant mixture was refluxed overnight, then cooled to room temperature. The mixture was concentrated and the residue was dissolved in CH2Cl2 (50 mL) and water (20 mL). Solid Na2CO3 was added ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Primary halide
C1CCNC1
null
c1ccccc1
HO-
C(Cl)(Cl)(Cl)Cl
null
null
COC(=O)c1ccc(C)c([N+](=O)[O-])c1.O=C1CCC(=O)N1Br>C(Cl)(Cl)(Cl)Cl>COC(=O)c1ccc(CBr)c([N+](=O)[O-])c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9689d5366eb44f93b0738e4b5c2d797b
COC(=O)c1ccc(CBr)c([N+](=O)[O-])c1.Cc1cccnc1C1CCCC(c2ncccc2C)N1>>COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c([N+](=O)[O-])c1
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.COC(C1=CC(=C(C=C1)CBr)[N+](=O)[O-])=O.CCN(C(C)C)C(C)C>>COC(C1=CC(=C(C=C1)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)[N+](=O)[O-])=O
Br[CH2:9][c:8]1[cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:34][c:30]1[N+:31](=[O:32])[O-:33].[NH:10]1[CH:11]([c:12]2[n:13][cH:14][cH:15][cH:16][c:17]2[CH3:18])[CH2:19][CH2:20][CH2:21][CH:22]1[c:23]1[n:24][cH:25][cH:26][cH:27][c:28]1[CH3:29]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH2:9][N:10]2[CH:11]([c:...
COC(=O)c1ccc(CBr)c([N+](=O)[O-])c1.Cc1cccnc1C1CCCC(c2ncccc2C)N1
COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c([N+](=O)[O-])c1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[#7;a:5]:[c:6]-[C:7](-[C:8])-[NH;D2;+0:9]-[C:10](-[c:11]:[#7;a:12])-[C:13]>>[#7;a:5]:[c:6]-[C:7](-[C:8])-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10](-[c:11]:[#7;a:12])-[C:13]
98.1
[{"value": 98.0, "product": "COC(C1=CC(=C(C=C1)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)[N+](=O)[O-])=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.1, "product": "COC(C1=CC(=C(C=C1)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)[N+](=O)[O-])=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: A solution of 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.829 g, 3.10 mmol), 4-bromomethyl-3-nitrobenzoic acid methyl ester (1.26 g, 4.61 mmol), KI (115 mg, 0.69 mmol), and DIPEA (1.20 mL, 6.89 mmol) in DMF (16 mL) was heated at 60° C. for 18 hours. Purification of th...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccccc1.c1ccncc1.C1CC[NH]CC1.c1ccncc1
HBr
CN(C)C=O
null
null
COC(=O)c1ccc(CBr)c([N+](=O)[O-])c1.Cc1cccnc1C1CCCC(c2ncccc2C)N1>CN(C)C=O>COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c([N+](=O)[O-])c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-caedbfd91ed74b8fa4184a2c95b7f89d
COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c([N+](=O)[O-])c1>>COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c(N)c1
COC(C1=CC(=C(C=C1)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)[N+](=O)[O-])=O>>COC(C1=CC(=C(C=C1)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)N)=O
O=[N+:31]([O-])[c:30]1[c:8]([CH2:9][N:10]2[CH:11]([c:12]3[n:13][cH:14][cH:15][cH:16][c:17]3[CH3:18])[CH2:19][CH2:20][CH2:21][CH:22]2[c:23]2[n:24][cH:25][cH:26][cH:27][c:28]2[CH3:29])[cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:32]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH2:9][N:10]2[CH:11]([c:12]3[n:13]...
COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c([N+](=O)[O-])c1
COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c(N)c1
null
[Pd]
CO.CCOC(=O)C
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
69
[{"value": 69.0, "product": "COC(C1=CC(=C(C=C1)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)N)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 69.0, "product": "COC(C1=CC(=C(C=C1)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)N)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: A solution of 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.829 g, 3.10 mmol), 4-bromomethyl-3-nitrobenzoic acid methyl ester (1.26 g, 4.61 mmol), KI (115 mg, 0.69 mmol), and DIPEA (1.20 mL, 6.89 mmol) in DMF (16 mL) was heated at 60° C. for 18 hours. Purification of th...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccncc1.C1CC[NH]CC1.c1ccncc1
Other
[Pd].CO.CCOC(=O)C
null
null
COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c([N+](=O)[O-])c1>[Pd].CO.CCOC(=O)C>COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)c(N)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5b98b66900a94a9a9fc3531729dcd456
COC(=O)c1ccccc1C.O=C1CCC(=O)N1Br>>COC(=O)c1ccccc1CBr
N(=NC1(CCCCC1)C#N)C1(CCCCC1)C#N.COC(C1=C(C=CC=C1)C)=O.BrN1C(CCC1=O)=O>>COC(C1=C(C=CC=C1)CBr)=O
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][cH:9][c:10]1[CH3:11].O=C1CCC(=O)N1[Br:12]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][cH:9][c:10]1[CH2:11][Br:12]
COC(=O)c1ccccc1C.O=C1CCC(=O)N1Br
COC(=O)c1ccccc1CBr
null
null
C(Cl)(Cl)(Cl)Cl
Functional Group Interconversion
Wohl-Ziegler bromination benzyl primary
45c0aca0d63a96f0092e6dded9c888827eaf6379dac179e1cefc99293896300a
08f5e7e34d3f321cce3e85421b38226d6240cca0939494ae61032d4f8405cf22
c1ccccc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[#8:2]-[C:3](=[O;D1;H0:4])-[c:5]:[c:6](-[CH3;D1;+0:7]):[c:8]>>[#8:2]-[C:3](=[O;D1;H0:4])-[c:5]:[c:6](-[CH2;D2;+0:7]-[Br;H0;D1;+0:1]):[c:8]
78
[{"value": 78.0, "product": "COC(C1=C(C=CC=C1)CBr)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.9, "product": "COC(C1=C(C=CC=C1)CBr)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 2-methyl-benzoic acid methyl ester (4.58 g, 30.5 mmol) in CCl4 (75 mL) was added N-bromosuccinimide (5.79 g, 32.5 mmol) followed by 1,1′-azobis(cyclohexanecarbonitrile) (1.42 g, 5.80 mmol). The resultant mixture was refluxed for 6 hours then cooled to room temperature, filtered through filter paper, an...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Primary halide
C1CCNC1
null
c1ccccc1
HO-
C(Cl)(Cl)(Cl)Cl
null
null
COC(=O)c1ccccc1C.O=C1CCC(=O)N1Br>C(Cl)(Cl)(Cl)Cl>COC(=O)c1ccccc1CBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ac3d2913dff2459bb6045f47cb02c8fc
CC(=O)c1ccccc1C.O=C1CCC(=O)N1Br.OCCO>>CC1(c2ccccc2CBr)OCCO1
BrN1C(CCC1=O)=O.CC1=C(C=CC=C1)C(C)=O.C(CO)O.N(=NC1(CCCCC1)C#N)C1(CCCCC1)C#N.O.C1(=CC=C(C=C1)S(=O)(=O)O)C>>BrCC1=C(C=CC=C1)C1(OCCO1)C
[CH3:1][C:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[CH3:9])=[O:11].O=C1CCC(=O)N1[Br:10].O[CH2:12][CH2:13][OH:14]>>[CH3:1][C:2]1([c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][Br:10])[O:11][CH2:12][CH2:13][O:14]1
CC(=O)c1ccccc1C.O=C1CCC(=O)N1Br.OCCO
CC1(c2ccccc2CBr)OCCO1
null
null
C1=CC=CC=C1.CCOCC
Heteroatom Alkylation and Arylation
OtherReaction
a600dedac1763c4f45af318938e18604b2fdb48d7ca40a6c88d35b0267d63357
2c0d9125c7e823dfb9df94c919dfb6803a7f1b063007b4bd723c966af137913c
c1ccc(C2OCCO2)cc1
O-[CH2;D2;+0:1]-[C:2]-[OH;D1;+0:3].O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:4].[C;D1;H3:5]-[C;H0;D3;+0:6](=[O;H0;D1;+0:7])-[c:8](:[c:9]):[c:10](-[CH3;D1;+0:11]):[c:12]>>[Br;H0;D1;+0:4]-[CH2;D2;+0:11]-[c:10](:[c:12]):[c:8](-[C;H0;D4;+0:6]1(-[C;D1;H3:5])-[O;H0;D2;+0:7]-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-1):[c:9]
80
[{"value": 80.0, "product": "BrCC1=C(C=CC=C1)C1(OCCO1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.5, "product": "BrCC1=C(C=CC=C1)C1(OCCO1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 2′-methyl-acetophenone (2.68 g, 20.0 mmol) in benzene (100 mL) was added ethylene glycol (2.0 mL, 35.9 mmol) followed by p-toluenesulfonic acid monohydrate (0.39 g, 2.10 mmol). The reaction flask was topped with a Dean-Stark trap, and the mixture was heated to reflux overnight. The mixture was cooled t...
10.6084/m9.figshare.5104873.v1
null
Ketone.Tertiary amide.Tertiary amide.Primary alcohol.Primary alcohol
Primary halide.Ether.Ether
C1CCNC1
C1COCO1
c1ccccc1.C1COCO1
HO-
C1=CC=CC=C1.CCOCC
null
null
CC(=O)c1ccccc1C.O=C1CCC(=O)N1Br.OCCO>C1=CC=CC=C1.CCOCC>CC1(c2ccccc2CBr)OCCO1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5a8d13c7819d4a7bbf64af0122245ff7
CC1(c2ccccc2CBr)OCCO1.Cc1cccnc1C1CCCC(c2ncccc2C)N1>>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccccc1C1(C)OCCO1
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.BrCC1=C(C=CC=C1)C1(OCCO1)C.CCN(C(C)C)C(C)C>>CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C=CC=C1)C1(OCCO1)C
Br[CH2:21][c:22]1[cH:23][cH:24][cH:25][cH:26][c:27]1[C:28]1([CH3:29])[O:30][CH2:31][CH2:32][O:33]1.[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([...
CC1(c2ccccc2CBr)OCCO1.Cc1cccnc1C1CCCC(c2ncccc2C)N1
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccccc1C1(C)OCCO1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(C2CCCC(c3ccccn3)N2Cc2ccccc2C2OCCO2)nc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[#7;a:5]:[c:6]-[C:7](-[C:8])-[NH;D2;+0:9]-[C:10](-[c:11]:[#7;a:12])-[C:13]>>[#7;a:5]:[c:6]-[C:7](-[C:8])-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10](-[c:11]:[#7;a:12])-[C:13]
90
[{"value": 90.0, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C=CC=C1)C1(OCCO1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.5, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C=CC=C1)C1(OCCO1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: A solution of 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.547 g, 2.04 mmol), 2-(2-bromomethyl-phenyl)-2-methyl-[1,3]dioxolane (1.03 g, 3.99 mmol), KI (73 mg, 0.42 mmol), and DIPEA (0.70 mL, 4.02 mmol) in DMF (10 mL) was heated at 60° C. for 24 hours. Purification of t...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1.C1COCO1
HBr
CN(C)C=O
null
null
CC1(c2ccccc2CBr)OCCO1.Cc1cccnc1C1CCCC(c2ncccc2C)N1>CN(C)C=O>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccccc1C1(C)OCCO1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a62703f2863846e6afd6ff32984ed4ec
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1ccc(CBr)cc1>>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.BrCC1=CC=C(C=C1)C#N.CCN(C(C)C)C(C)C>>CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=CC=C(C#N)C=C1
[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1.Br[CH2:21][c:22]1[cH:23][cH:24][c:25]([C:26]#[N:27])[cH:28][cH:29]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:1...
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1ccc(CBr)cc1
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[#7;a:5]:[c:6]-[C:7](-[C:8])-[NH;D2;+0:9]-[C:10](-[c:11]:[#7;a:12])-[C:13]>>[#7;a:5]:[c:6]-[C:7](-[C:8])-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10](-[c:11]:[#7;a:12])-[C:13]
94.3
[{"value": 94.0, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=CC=C(C#N)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 94.3, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=CC=C(C#N)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: A solution of 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.502 g, 1.83 mmol), α-bromo-p-tolunitrile (0.538 g, 2.75 mmol), KI (65 mg, 0.40 mmol), and DIPEA (0.72 mL, 4.13 mmol) in DMF (9 mL) was heated at 60° C. for 16 hours. Purification of the crude material by column...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1
HBr
CN(C)C=O
null
null
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1ccc(CBr)cc1>CN(C)C=O>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a362150b2d8c47d9b50a079bd6b19fe2
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1cccc(CBr)c1>>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1cccc(C#N)c1
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.BrCC1=CC(=CC=C1)C#N.CCN(C(C)C)C(C)C>>CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC=1C=C(C#N)C=CC1
[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1.Br[CH2:21][c:22]1[cH:23][cH:24][cH:25][c:26]([C:27]#[N:28])[cH:29]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:1...
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1cccc(CBr)c1
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1cccc(C#N)c1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[#7;a:5]:[c:6]-[C:7](-[C:8])-[NH;D2;+0:9]-[C:10](-[c:11]:[#7;a:12])-[C:13]>>[#7;a:5]:[c:6]-[C:7](-[C:8])-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10](-[c:11]:[#7;a:12])-[C:13]
75.4
[{"value": 75.0, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC=1C=C(C#N)C=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.4, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC=1C=C(C#N)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: A solution of 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (0.414 g, 1.55 mmol), α-bromo-m-tolunitrile (0.466 g, 2.38 mmol), KI (53 mg, 0.32 mmol), and DIPEA (0.55 mL, 3.16 mmol) in DMF (8 mL) was heated at 60° C. for 18 hours. Purification of the crude material by column...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1
HBr
CN(C)C=O
null
null
Cc1cccnc1C1CCCC(c2ncccc2C)N1.N#Cc1cccc(CBr)c1>CN(C)C=O>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1cccc(C#N)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ec4f0cfe78cd47c59b3f817a1665ac00
COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)cc1>>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C(=O)O)cc1
COC(C1=CC=C(C=C1)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C)=O.O.[OH-].[Na+].Cl>>CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=CC=C(C(=O)O)C=C1
C[O:28][C:26]([c:25]1[cH:24][cH:23][c:22]([CH2:21][N:20]2[CH:8]([c:7]3[c:2]([CH3:1])[cH:3][cH:4][cH:5][n:6]3)[CH2:9][CH2:10][CH2:11][CH:12]2[c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[cH:30][cH:29]1)=[O:27]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:1...
COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)cc1
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C(=O)O)cc1
null
null
CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4]>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4]
108.5
[{"value": 108.5, "product": "CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=CC=C(C(=O)O)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 4-(3,3″-dimethyl-3′,4′,5′,6′-tetrahydro-2′H-[2,2′;6′,2″]terpyridin-1′-ylmethyl)-benzoic acid methyl ester (0.420 g, 1.01 mmol) in MeOH (5 mL) was added water (5 mL) and solid NaOH (0.448 g, 11.21 mmol). The resultant mixture was heated to reflux overnight then cooled to room temperature. The mixture wa...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1
Other
CO
null
null
COC(=O)c1ccc(CN2C(c3ncccc3C)CCCC2c2ncccc2C)cc1>CO>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C(=O)O)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-53957fe214f7449597c1405a3df69165
CCOC(=O)CCCCCBr.Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1>>CCOC(=O)CCCCCN1[C@@H](c2ncccc2C)CCC[C@H]1c1ncccc1C
CC=1C(=NC=CC1)[C@@H]1N[C@@H](CCC1)C1=NC=CC=C1C.C(C)OC(CCCCCBr)=O.CCN(C(C)C)C(C)C>>C(C)OC(CCCCCN1[C@H](CCC[C@H]1C1=NC=CC=C1C)C1=NC=CC=C1C)=O
Br[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][C:4]([O:3][CH2:2][CH3:1])=[O:5].[NH:11]1[C@H:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[CH2:20][CH2:21][CH2:22][C@@H:23]1[c:24]1[n:25][cH:26][cH:27][cH:28][c:29]1[CH3:30]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][N:11]1[C@@H:12]([c:13]2[n:14...
CCOC(=O)CCCCCBr.Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1
CCOC(=O)CCCCCN1[C@@H](c2ncccc2C)CCC[C@H]1c1ncccc1C
null
null
CC#N
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc([C@@H]2CCC[C@H](c3ccccn3)N2)nc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7;a:4]:[c:5]-[C:6](-[C:7])-[NH;D2;+0:8]-[C:9](-[c:10]:[#7;a:11])-[C:12]>>[#7;a:4]:[c:5]-[C:6](-[C:7])-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3])-[C:9](-[c:10]:[#7;a:11])-[C:12]
90.2
[{"value": 90.0, "product": "C(C)OC(CCCCCN1[C@H](CCC[C@H]1C1=NC=CC=C1C)C1=NC=CC=C1C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.2, "product": "C(C)OC(CCCCCN1[C@H](CCC[C@H]1C1=NC=CC=C1C)C1=NC=CC=C1C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
23
HOUR
A solution of (2′R,6′S)-3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (308 mg, 1.15 mmol), 6-bromo-hexanoic acid ethyl ester (283 mg, 1.27 mmol), DIPEA (260 μL, 1.49 mmol) and KI (10 mg, 0.060 mmol) in CH3CN (12 mL) was warmed to 60° C. and stirred for 23 h according to General Procedure A. Purifica...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccncc1.c1ccncc1
HBr
CC#N
null
23
CCOC(=O)CCCCCBr.Cc1cccnc1[C@@H]1CCC[C@H](c2ncccc2C)N1>CC#N>CCOC(=O)CCCCCN1[C@@H](c2ncccc2C)CCC[C@H]1c1ncccc1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-4a8d6f2890094fde847fcfbd5892dbb6
COC(=O)c1cc(C#N)ccc1CBr.Clc1cccnc1C1CCCC(c2ncccc2Cl)N1>>COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2Cl)CCCC1c1ncccc1Cl
ClC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1Cl.COC(C1=C(C=CC(=C1)C#N)CBr)=O.CCN(C(C)C)C(C)C>>COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1Cl)C1=NC=CC=C1Cl)=O
Br[CH2:13][c:12]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:6][c:7]([C:8]#[N:9])[cH:10][cH:11]1.[NH:14]1[CH:15]([c:16]2[n:17][cH:18][cH:19][cH:20][c:21]2[Cl:22])[CH2:23][CH2:24][CH2:25][CH:26]1[c:27]1[n:28][cH:29][cH:30][cH:31][c:32]1[Cl:33]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([C:8]#[N:9])[cH:10][cH:11][c:12]1[CH2:13]...
COC(=O)c1cc(C#N)ccc1CBr.Clc1cccnc1C1CCCC(c2ncccc2Cl)N1
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2Cl)CCCC1c1ncccc1Cl
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7].[#7;a:8]:[c:9]-[C:10](-[C:11])-[NH;D2;+0:12]-[C:13](-[c:14]:[#7;a:15])-[C:16]>>[#7;a:8]:[c:9]-[C:10](-[C:11])-[N;H0;D3;+0:12](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7])-[C:13](-[c:14]:[#7;a:15])-[C:16]
82.3
[{"value": 82.0, "product": "COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1Cl)C1=NC=CC=C1Cl)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.3, "product": "COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1Cl)C1=NC=CC=C1Cl)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: 3,3″-dichloro-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (304 mg, 0.987 mmol), 2-bromomethyl-5-cyano-benzoic acid methyl ester (351 mg, 1.38 mmol), KI (32.7 mg, 0.197 mmol), DIPEA (0.34 mL, 1.97 mmol), and DMF (5 mL) were stirred at 60° C. for 3 h. Purification of the crude material ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccccc1.c1ccncc1.C1CC[NH]CC1.c1ccncc1
HBr
CN(C)C=O
null
null
COC(=O)c1cc(C#N)ccc1CBr.Clc1cccnc1C1CCCC(c2ncccc2Cl)N1>CN(C)C=O>COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2Cl)CCCC1c1ncccc1Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-65a609bf873e4f87ae8f56f5fee6f767
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2Cl)CCCC1c1ncccc1Cl>>N#Cc1ccc(CN2C(c3ncccc3Cl)CCCC2c2ncccc2Cl)c(CO)c1
COC(C1=C(C=CC(=C1)C#N)CN1C(CCCC1C1=NC=CC=C1Cl)C1=NC=CC=C1Cl)=O.[Li+].[BH4-]>>ClC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1Cl)CC1=C(C=C(C#N)C=C1)CO
CO[C:29]([c:28]1[c:6]([CH2:7][N:8]2[CH:9]([c:10]3[n:11][cH:12][cH:13][cH:14][c:15]3[Cl:16])[CH2:17][CH2:18][CH2:19][CH:20]2[c:21]2[n:22][cH:23][cH:24][cH:25][c:26]2[Cl:27])[cH:5][cH:4][c:3]([C:2]#[N:1])[cH:31]1)=[O:30]>>[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][N:8]2[CH:9]([c:10]3[n:11][cH:12][cH:13][cH:14][c:15]3[Cl:...
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2Cl)CCCC1c1ncccc1Cl
N#Cc1ccc(CN2C(c3ncccc3Cl)CCCC2c2ncccc2Cl)c(CO)c1
null
null
CO.[OH-].[Na+].C1CCOC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3](:[c:4]):[c:5]>>[OH;D1;+0:2]-[CH2;D2;+0:1]-[c:3](:[c:4]):[c:5]
99.6
[{"value": 99.6, "product": "ClC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1Cl)CC1=C(C=C(C#N)C=C1)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3.5
HOUR
To a cold (0° C.) solution of 5-cyano-2-(3,3″-dichloro-3′,4′,5′,6′-tetrahydro-2′H-[2,2′;6′,2″]terpyridin-1′-ylmethyl)-benzoic acid methyl ester (391 mg, 0.813 mmol) in THF (4 mL) and MeOH (4 mL) was added LiBH4 (88 mg, 4.1 mmol), and the mixture was warmed to room temperature and stirred for 3.5 h. The mixture was dilu...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccccc1.c1ccncc1.C1CC[NH]CC1.c1ccncc1
Other
CO.[OH-].[Na+].C1CCOC1
null
3.5
COC(=O)c1cc(C#N)ccc1CN1C(c2ncccc2Cl)CCCC1c1ncccc1Cl>CO.[OH-].[Na+].C1CCOC1>N#Cc1ccc(CN2C(c3ncccc3Cl)CCCC2c2ncccc2Cl)c(CO)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5e18d3597c814e759d3eb303dda0f79f
BrCCCBr.c1c[nH]cn1>>BrCCCn1ccnc1
N1C=NC=C1.BrCCCBr.[H-].[Na+]>>BrCCCN1C=NC=C1
Br[CH2:4][CH2:3][CH2:2][Br:1].[nH:5]1[cH:6][cH:7][n:8][cH:9]1>>[Br:1][CH2:2][CH2:3][CH2:4][n:5]1[cH:6][cH:7][n:8][cH:9]1
BrCCCBr.c1c[nH]cn1
BrCCCn1ccnc1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
b9d84e1ee028da6e8c5d8924d45fbf8f3755d9adc2caf0035bd5ed7f30f5ee03
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
c1c[nH]cn1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7;a:4]1:[c:5]:[c:6]:[nH;D2;+0:7]:[c:8]:1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:7]1:[c:6]:[c:5]:[#7;a:4]:[c:8]:1
30
[{"value": 30.0, "product": "BrCCCN1C=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a stirred solution of imidazole (500 mg, 7.35 mmol) and 1,3-dibromopropane (2.2 mL, 22.0) in THF (35 mL) was added 60% NaH (356 mg, 8.82 mmol), and the resultant mixture was refluxed for 1 h and stirred at room temperature overnight. The mixture was quenched with H2O (25 mL) and diluted with CH2Cl2 (40 mL). The aque...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1c[nH]cn1
c1c[nH]cn1
c1c[nH]cn1
HBr
C1CCOC1
null
8
BrCCCBr.c1c[nH]cn1>C1CCOC1>BrCCCn1ccnc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9a2add3353b24f71a4bf49219117e507
BrCCCn1ccnc1.Cc1cccnc1C1CCCC(c2ncccc2C)N1>>Cc1cccnc1C1CCCC(c2ncccc2C)N1CCCn1ccnc1
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.BrCCCN1C=NC=C1.CCN(C(C)C)C(C)C>>N1(C=NC=C1)CCCN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C
Br[CH2:21][CH2:22][CH2:23][n:24]1[cH:25][cH:26][n:27][cH:28]1.[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:1...
BrCCCn1ccnc1.Cc1cccnc1C1CCCC(c2ncccc2C)N1
Cc1cccnc1C1CCCC(c2ncccc2C)N1CCCn1ccnc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(C2CCCC(c3ccccn3)N2CCCn2ccnc2)nc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7;a:4]:[c:5]-[C:6](-[C:7])-[NH;D2;+0:8]-[C:9](-[c:10]:[#7;a:11])-[C:12]>>[#7;a:4]:[c:5]-[C:6](-[C:7])-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3])-[C:9](-[c:10]:[#7;a:11])-[C:12]
38
[{"value": 38.0, "product": "N1(C=NC=C1)CCCN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 37.5, "product": "N1(C=NC=C1)CCCN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using General Procedure A: 3,3″-dimethyl-1′,2′,3′,4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (91.3 mg, 0.341 mmol), 1-(3-bromo-propyl)-1H-imidazole (129 mg, 0.680 mmol), KI (5.6 mg, 0.034 mmol), DIPEA (0.18 mL, 1.02 mmol), and DMF (3.4 mL) were stirred at 60° C. overnight. Purification of the crude material by flash ch...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1c[nH]cn1
HBr
CN(C)C=O
null
null
BrCCCn1ccnc1.Cc1cccnc1C1CCCC(c2ncccc2C)N1>CN(C)C=O>Cc1cccnc1C1CCCC(c2ncccc2C)N1CCCn1ccnc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-453460d0a36d41198be5545bdce21d62
BrCCCCBr.c1c[nH]cn1>>BrCCCCn1ccnc1
N1C=NC=C1.BrCCCCBr.[H-].[Na+]>>BrCCCCN1C=NC=C1
Br[CH2:5][CH2:4][CH2:3][CH2:2][Br:1].[nH:6]1[cH:7][cH:8][n:9][cH:10]1>>[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][n:6]1[cH:7][cH:8][n:9][cH:10]1
BrCCCCBr.c1c[nH]cn1
BrCCCCn1ccnc1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
b9d84e1ee028da6e8c5d8924d45fbf8f3755d9adc2caf0035bd5ed7f30f5ee03
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
c1c[nH]cn1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7;a:4]1:[c:5]:[nH;D2;+0:6]:[c:7]:[c:8]:1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:6]1:[c:5]:[#7;a:4]:[c:8]:[c:7]:1
null
[]
null
null
8
HOUR
To a stirred solution of imidazole (500 mg, 7.35 mmol) and 1,4-dibromobutane (2.6 mL, 22.0) in THF (50 mL) was added 60% NaH (356 mg, 8.81 mmol), and the resultant mixture was refluxed for 2 h and stirred at room temperature overnight. The mixture was quenched with H2O (50 mL) and diluted with CH2Cl2 (75 mL). The aqueo...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1c[nH]cn1
c1c[nH]cn1
c1c[nH]cn1
HBr
C1CCOC1
null
8
BrCCCCBr.c1c[nH]cn1>C1CCOC1>BrCCCCn1ccnc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e6270c35b1aa4c4d8815b6b30c1cf727
BrCCCCn1ccnc1.Cc1cccnc1C1CCCC(c2ncccc2C)N1>>Cc1cccnc1C1CCCC(c2ncccc2C)N1CCCCn1ccnc1
CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C.BrCCCCN1C=NC=C1.CCN(C(C)C)C(C)C>>N1(C=NC=C1)CCCCN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C
Br[CH2:21][CH2:22][CH2:23][CH2:24][n:25]1[cH:26][cH:27][n:28][cH:29]1.[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH...
BrCCCCn1ccnc1.Cc1cccnc1C1CCCC(c2ncccc2C)N1
Cc1cccnc1C1CCCC(c2ncccc2C)N1CCCCn1ccnc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(C2CCCC(c3ccccn3)N2CCCCn2ccnc2)nc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[#7;a:4]:[c:5]-[C:6](-[C:7])-[NH;D2;+0:8]-[C:9](-[c:10]:[#7;a:11])-[C:12]>>[#7;a:4]:[c:5]-[C:6](-[C:7])-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2]-[C:3])-[C:9](-[c:10]:[#7;a:11])-[C:12]
34.2
[{"value": 34.0, "product": "N1(C=NC=C1)CCCCN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 34.2, "product": "N1(C=NC=C1)CCCCN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a stirred solution of imidazole (500 mg, 7.35 mmol) and 1,4-dibromobutane (2.6 mL, 22.0) in THF (50 mL) was added 60% NaH (356 mg, 8.81 mmol), and the resultant mixture was refluxed for 2 h and stirred at room temperature overnight. The mixture was quenched with H2O (50 mL) and diluted with CH2Cl2 (75 mL). The aqueo...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1c[nH]cn1
HBr
CN(C)C=O
null
null
BrCCCCn1ccnc1.Cc1cccnc1C1CCCC(c2ncccc2C)N1>CN(C)C=O>Cc1cccnc1C1CCCC(c2ncccc2C)N1CCCCn1ccnc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b6e38debdb4e4f89bdadcddf63a58b91
CO.O=C(O)Cc1c[nH]cn1>>COC(=O)Cc1c[nH]cn1
Cl.N1C=NC(=C1)CC(=O)O.S(O)(O)(=O)=O.CO>>COC(CC=1N=CNC1)=O
[CH3:1][OH:2].O[C:3](=[O:4])[CH2:5][c:6]1[cH:7][nH:8][cH:9][n:10]1>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][c:6]1[cH:7][nH:8][cH:9][n:10]1
CO.O=C(O)Cc1c[nH]cn1
COC(=O)Cc1c[nH]cn1
null
null
null
Protection
Esterification of Carboxylic Acids
9cecdbd189c6f9c3648521d17154d013842a5498de4e76e65efb1d842973340b
af0b8064f2e82ebe66c4c29d2391785ac1b993104265ccdc4d67ca79e36fa3c8
c1c[nH]cn1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4](:[#7;a:5]):[c:6]:[#7;a:7].[C;D1;H3:8]-[OH;D1;+0:9]>>[#7;a:5]:[c:4](-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[O;H0;D2;+0:9]-[C;D1;H3:8]):[c:6]:[#7;a:7]
66
[{"value": 66.0, "product": "COC(CC=1N=CNC1)=O", "details": "PERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
To a solution of 4-imidazoleacetic acid hydrochloride (499 mg, 3.07 mmol) in MeOH (10 mL) was added concentrated sulfuric acid (1 mL) and the mixture was heated to 80° C. overnight. Then the mixture was cooled and concentrated. The residue was dissolved in CH2Cl2 (30 mL) and washed with saturated NaHCO3 (30 mL). The aq...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Methanol
Ester
null
null
c1c[nH]cn1
HO-
null
80
null
CO.O=C(O)Cc1c[nH]cn1>>COC(=O)Cc1c[nH]cn1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8e7597cbdb5847fba435581e46e3fceb
CO.Cc1ccc(F)cc1C(=O)O>>COC(=O)c1cc(F)ccc1C
FC=1C=CC(=C(C(=O)O)C1)C.CO.OS(=O)(=O)O>>COC(C1=C(C=CC(=C1)F)C)=O
[CH3:1][OH:2].O[C:3](=[O:4])[c:5]1[cH:6][c:7]([F:8])[cH:9][cH:10][c:11]1[CH3:12]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([F:8])[cH:9][cH:10][c:11]1[CH3:12]
CO.Cc1ccc(F)cc1C(=O)O
COC(=O)c1cc(F)ccc1C
null
null
null
Protection
Esterification of Carboxylic Acids
9cecdbd189c6f9c3648521d17154d013842a5498de4e76e65efb1d842973340b
af0b8064f2e82ebe66c4c29d2391785ac1b993104265ccdc4d67ca79e36fa3c8
c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C;D1;H3:6]-[OH;D1;+0:7]>>[C;D1;H3:6]-[O;H0;D2;+0:7]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
78
[{"value": 78.0, "product": "COC(C1=C(C=CC(=C1)F)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
5-Fluoro-2-methyl-benzoic acid (0.29 g, 1.9 mmol) was dissolved in anhydrous MeOH (7 mL) and c. H2SO4 (0.12 mL, 2.3 mmol) was added, heating to reflux for 16 hours. The solution was cooled to room temperature and partitioned between EtOAc (15 mL) and brine (10 mL). After separating, the aqueous phase was extracted with...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Methanol
Ester
null
null
c1ccccc1
HO-
null
null
null
CO.Cc1ccc(F)cc1C(=O)O>>COC(=O)c1cc(F)ccc1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c4ce1ab8900c4a21ace0be056038e3b9
Cc1ccc(S(=O)(=O)Cl)cc1.O=Cc1ncc[nH]1>>Cc1ccc(S(=O)(=O)n2ccnc2C=O)cc1
N1C(=NC=C1)C=O.CCN(CC)CC.S(=O)(=O)(C1=CC=C(C)C=C1)Cl>>C1(=CC=C(C=C1)S(=O)(=O)N1C(=NC=C1)C=O)C
Cl[S:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:17][cH:16]1)(=[O:7])=[O:8].[nH:9]1[cH:10][cH:11][n:12][c:13]1[CH:14]=[O:15]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[n:9]2[cH:10][cH:11][n:12][c:13]2[CH:14]=[O:15])[cH:16][cH:17]1
Cc1ccc(S(=O)(=O)Cl)cc1.O=Cc1ncc[nH]1
Cc1ccc(S(=O)(=O)n2ccnc2C=O)cc1
null
null
C(Cl)Cl
Acylation
OtherReaction
9d95b3f7a94155c15253f03a3d139421fdad476c6138a59a600798d164b552ae
b7cf703ff8ec1befb0c6e5230d29d7904f3e22c3606b15633c7e7a7fc4abca48
O=S(=O)(c1ccccc1)n1ccnc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[O;D1;H0:7]=[C:8]-[c:9]1:[#7;a:10]:[c:11]:[c:12]:[nH;D2;+0:13]:1>>[O;D1;H0:7]=[C:8]-[c:9]1:[#7;a:10]:[c:11]:[c:12]:[n;H0;D3;+0:13]:1-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
58.2
[{"value": 58.0, "product": "C1(=CC=C(C=C1)S(=O)(=O)N1C(=NC=C1)C=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 58.2, "product": "C1(=CC=C(C=C1)S(=O)(=O)N1C(=NC=C1)C=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a suspension of 2-imidazolecarboxaldehyde (1.01 g, 10.51 mmol) in CH2Cl2 (25 mL) was added Et3N (2.9 mL, 21.02 mmol) and tosyl chloride (3.01 g, 15.77 mmol) and the reaction mixture was heated to reflux overnight. Then the mixture was cooled and washed with saturated NH4Cl (4×30 mL). The organic layer was dried (MgS...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Sulfonyl halide
Tosylate
c1c[nH]cn1
c1ncc[nH]1
c1ccccc1.c1ncc[nH]1
HCl
C(Cl)Cl
null
null
Cc1ccc(S(=O)(=O)Cl)cc1.O=Cc1ncc[nH]1>C(Cl)Cl>Cc1ccc(S(=O)(=O)n2ccnc2C=O)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-1cccd055a88448d3bbd9dd847eaf0a80
Cc1ccc(S(=O)(=O)n2ccnc2C=O)cc1>>Cc1ccc(S(=O)(=O)n2ccnc2CO)cc1
C1(=CC=C(C=C1)S(=O)(=O)N1C(=NC=C1)C=O)C.C(=O)(C(F)(F)F)O>>C1(=CC=C(C=C1)S(=O)(=O)N1C(=NC=C1)CO)C
[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[n:9]2[cH:10][cH:11][n:12][c:13]2[CH:14]=[O:15])[cH:16][cH:17]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[n:9]2[cH:10][cH:11][n:12][c:13]2[CH2:14][OH:15])[cH:16][cH:17]1
Cc1ccc(S(=O)(=O)n2ccnc2C=O)cc1
Cc1ccc(S(=O)(=O)n2ccnc2CO)cc1
null
null
C(Cl)Cl
Reduction
Reduction of aldehydes and ketones to alcohols
e7895795cd3f75445716c94697823c5929dcd4b5344525875fe75d36bca2f9d7
21bb81d5469aaaca71ab12c186bea4016451717fad8780cf288858a7d8fbc55a
O=S(=O)(c1ccccc1)n1ccnc1
[#16:1]-[#7;a:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:1-[CH;D2;+0:7]=[O;H0;D1;+0:8]>>[#16:1]-[#7;a:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:1-[CH2;D2;+0:7]-[OH;D1;+0:8]
36
[{"value": 36.0, "product": "C1(=CC=C(C=C1)S(=O)(=O)N1C(=NC=C1)CO)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 35.7, "product": "C1(=CC=C(C=C1)S(=O)(=O)N1C(=NC=C1)CO)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of the above aldehyde (1.53 g, 6.11 mmol) in CH2Cl2 (50 mL) at 0° C. was added TFA (5 mL) as described in J. Med. Chem. (1997) 40:2196. Purification by flash column chromatography using EtOAc/hexane (1:1) afforded [1-(toluene-4-sulfonyl)-1H-imidazol-2-yl]-methanol as a white solid (0.55 g, 36%). 1H NMR (C...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Primary alcohol
null
null
c1ccccc1.c1ncc[nH]1
null
C(Cl)Cl
null
null
Cc1ccc(S(=O)(=O)n2ccnc2C=O)cc1>C(Cl)Cl>Cc1ccc(S(=O)(=O)n2ccnc2CO)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-00b8ffdb5a4049e29a7c27475c4f58f0
BrC(Br)(Br)Br.Cc1ccc(S(=O)(=O)n2ccnc2CO)cc1>>Cc1ccc(S(=O)(=O)n2ccnc2CBr)cc1
C1(=CC=C(C=C1)S(=O)(=O)N1C(=NC=C1)CO)C.C(Br)(Br)(Br)Br.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>BrCC=1N(C=CN1)S(=O)(=O)C1=CC=C(C=C1)C
BrC(Br)(Br)[Br:15].O[CH2:14][c:13]1[n:9]([S:6]([c:5]2[cH:4][cH:3][c:2]([CH3:1])[cH:17][cH:16]2)(=[O:7])=[O:8])[cH:10][cH:11][n:12]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[n:9]2[cH:10][cH:11][n:12][c:13]2[CH2:14][Br:15])[cH:16][cH:17]1
BrC(Br)(Br)Br.Cc1ccc(S(=O)(=O)n2ccnc2CO)cc1
Cc1ccc(S(=O)(=O)n2ccnc2CBr)cc1
null
null
C(Cl)Cl
Functional Group Interconversion
Appel reaction
752e1807cd47d8316010cc3f92eab16c5a89ffb844d9514fcae469ba993c78dd
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
O=S(=O)(c1ccccc1)n1ccnc1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[c:3]1:[#7;a:4]:[c:5]:[c:6]:[#7;a:7]:1-[#16:8]>>[#16:8]-[#7;a:7]1:[c:6]:[c:5]:[#7;a:4]:[c:3]:1-[CH2;D2;+0:2]-[Br;H0;D1;+0:1]
45.3
[{"value": 45.0, "product": "BrCC=1N(C=CN1)S(=O)(=O)C1=CC=C(C=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 45.3, "product": "BrCC=1N(C=CN1)S(=O)(=O)C1=CC=C(C=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of the above alcohol (0.55 g, 2.17 mmol) and CBr4 (1.08 g, 3.26 mmol) in CH2Cl2 (25 mL) at 0° C. was added a solution of triphenylphosphine (0.68 g, 2.60 mmol) in CH2Cl2 (10 mL) as described in J. Med. Chem. (1997) 40, 14:2196. Purification by flash column chromatography using 25% EtOAc/hexanes afforded 2...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
null
null
c1ccccc1.c1ncc[nH]1
HBr
C(Cl)Cl
null
null
BrC(Br)(Br)Br.Cc1ccc(S(=O)(=O)n2ccnc2CO)cc1>C(Cl)Cl>Cc1ccc(S(=O)(=O)n2ccnc2CBr)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-29461549a9f644e5a4b0db020a8a3439
CCOC(=O)C1CCN(S(=O)(=O)c2ccc(C)cc2)CC1>>Cc1ccc(S(=O)(=O)N2CCC(CO)CC2)cc1
C(C)OC(=O)C1CCN(CC1)S(=O)(=O)C1=CC=C(C=C1)C.[H-].[H-].[H-].[H-].[Li+].[Al+3].C1CCOC1>>C1(=CC=C(C=C1)S(=O)(=O)N1CCC(CC1)CO)C
CCO[C:13]([CH:12]1[CH2:11][CH2:10][N:9]([S:6]([c:5]2[cH:4][cH:3][c:2]([CH3:1])[cH:18][cH:17]2)(=[O:7])=[O:8])[CH2:16][CH2:15]1)=[O:14]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[N:9]2[CH2:10][CH2:11][CH:12]([CH2:13][OH:14])[CH2:15][CH2:16]2)[cH:17][cH:18]1
CCOC(=O)C1CCN(S(=O)(=O)c2ccc(C)cc2)CC1
Cc1ccc(S(=O)(=O)N2CCC(CO)CC2)cc1
null
null
C(Cl)Cl
Functional Group Interconversion
Reduction of ester to primary alcohol
cd99347e3144bc4f081bc664a4bc5a11d1e392f7cea47a5adad92bcd498ccf56
a2b5cf843cfeb048c76ac4cbf0bd8ccab026fcad80259b78e012cdb6ac2f5934
O=S(=O)(c1ccccc1)N1CCCCC1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3](-[C:4])-[C:5]>>[C:4]-[C:3](-[CH2;D2;+0:1]-[OH;D1;+0:2])-[C:5]
100
[{"value": 100.0, "product": "C1(=CC=C(C=C1)S(=O)(=O)N1CCC(CC1)CO)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.1, "product": "C1(=CC=C(C=C1)S(=O)(=O)N1CCC(CC1)CO)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
To a solution of the above ester (1.29 g, 4.79 mmol) in CH2Cl2 (20 mL) at 0° C. was added a solution of LiAlH4 in THF (1.0 M, 13.9 mL, 13.87 mmol) and the mixture was heated to reflux. After 1 h, the mixture was cooled back down to 0° C. and quenched with H2O (0.51 mL), 15% NaOH (0.51 mL), and H2O (1.53 mL). After stir...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccccc1.C1CC[NH]CC1
HO-
C(Cl)Cl
0
1
CCOC(=O)C1CCN(S(=O)(=O)c2ccc(C)cc2)CC1>C(Cl)Cl>Cc1ccc(S(=O)(=O)N2CCC(CO)CC2)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c97fed26492e4b758945b9c149c8318a
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1CO>>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(CN)cc1CO.[NH4+].[OH-]
CC=1C(=NC=CC1)C1N(C(CCC1)C1=NC=CC=C1C)CC1=C(C=C(C#N)C=C1)CO>>[NH4+].[OH-].NCC=1C=CC(=C(C1)CO)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C
[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[N:20]1[CH2:21][c:22]1[cH:23][cH:24][c:25]([C:26]#[N:27])[cH:28][c:29]1[CH2:30][OH:31]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][c...
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1CO
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(CN)cc1CO.[NH4+].[OH-]
null
null
CO
Functional Group Interconversion
Reduction of nitrile to amine
3b047a13c16a607c445b1c419e256808e8c9a0097d8fb9efd4e7970deb782b70
2882e57127fc469aa16ca9a2fd53388b6d97c74c76c010e6eb01be5726f46aa5
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[NH2;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]
175.2
[{"value": 88.0, "product": "NCC=1C=CC(=C(C1)CO)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 175.2, "product": "NCC=1C=CC(=C(C1)CO)CN1C(CCCC1C1=NC=CC=C1C)C1=NC=CC=C1C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2.5
HOUR
To a solution of 4-(3,3″-dimethyl-3′,4′,5′,6′-tetrahydro-2′H-[2,2′;6′,2″]terpyridin-1′-ylmethyl)-3-hydroxymethyl-benzonitrile (0.610 g, 1.48 mmol) dissolved in MeOH (12 mL) ammonia gas was bubbled for 10 minutes. A pre-washed mixture of Raney Nickel (˜1.5 grams) was added to the nitrile and the mixture was shaken on th...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1
Other
CO
null
2.5
Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(C#N)cc1CO>CO>Cc1cccnc1C1CCCC(c2ncccc2C)N1Cc1ccc(CN)cc1CO.[NH4+].[OH-]
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-bbe1a5193e8f44d29aac70cb11d77962
Cc1cnc(C2CCCC(c3ncc(C)cc3C)N2Cc2ccc(C#N)cc2CO)c(C)c1>>Cc1cnc(C2CCCC(c3ncc(C)cc3C)N2Cc2ccc(CN)cc2CO)c(C)c1.[NH4+].[OH-]
OCC=1C=C(C#N)C=CC1CN1C(CCCC1C1=NC=C(C=C1C)C)C1=NC=C(C=C1C)C>>[NH4+].[OH-].NCC=1C=CC(=C(C1)CO)CN1C(CCCC1C1=NC=C(C=C1C)C)C1=NC=C(C=C1C)C
[CH3:1][c:2]1[cH:3][n:4][c:5]([CH:6]2[CH2:7][CH2:8][CH2:9][CH:10]([c:11]3[n:12][cH:13][c:14]([CH3:15])[cH:16][c:17]3[CH3:18])[N:19]2[CH2:20][c:21]2[cH:22][cH:23][c:24]([C:25]#[N:26])[cH:27][c:28]2[CH2:29][OH:30])[c:31]([CH3:32])[cH:33]1>>[CH3:1][c:2]1[cH:3][n:4][c:5]([CH:6]2[CH2:7][CH2:8][CH2:9][CH:10]([c:11]3[n:12][cH...
Cc1cnc(C2CCCC(c3ncc(C)cc3C)N2Cc2ccc(C#N)cc2CO)c(C)c1
Cc1cnc(C2CCCC(c3ncc(C)cc3C)N2Cc2ccc(CN)cc2CO)c(C)c1.[NH4+].[OH-]
null
null
CO
Functional Group Interconversion
Reduction of nitrile to amine
3b047a13c16a607c445b1c419e256808e8c9a0097d8fb9efd4e7970deb782b70
2882e57127fc469aa16ca9a2fd53388b6d97c74c76c010e6eb01be5726f46aa5
c1ccc(CN2C(c3ccccn3)CCCC2c2ccccn2)cc1
[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[NH2;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]
196
[{"value": 99.0, "product": "NCC=1C=CC(=C(C1)CO)CN1C(CCCC1C1=NC=C(C=C1C)C)C1=NC=C(C=C1C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 196.0, "product": "NCC=1C=CC(=C(C1)CO)CN1C(CCCC1C1=NC=C(C=C1C)C)C1=NC=C(C=C1C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a solution of 3-hydroxymethyl-4-(3,5,3″,5″-tetramethyl-3′,4′,5′,6′-tetrahydro-2′H-[2,2′;6′,2″]terpyridin-1′-ylmethyl)-benzonitrile (0.060 g, 0.14 mmol) dissolved in MeOH (7 mL) ammonia gas was bubbled for 10 minutes. A pre-washed mixture of Raney Nickel (˜0.5 gram) was added to the nitrile and the mixture was shaken...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
c1ccncc1.C1CC[NH]CC1.c1ccncc1.c1ccccc1
Other
CO
null
2
Cc1cnc(C2CCCC(c3ncc(C)cc3C)N2Cc2ccc(C#N)cc2CO)c(C)c1>CO>Cc1cnc(C2CCCC(c3ncc(C)cc3C)N2Cc2ccc(CN)cc2CO)c(C)c1.[NH4+].[OH-]
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-f7865eb4f1c34d4ab6f6b5c5db4bdf57
CC(C)(C)OC(=O)N1CC(CN)C1.O=[N+]([O-])c1ccccc1S(=O)(=O)Cl>>O=[N+]([O-])c1ccccc1S(=O)(=O)N1CC(CO)C1
C(=O)(C(F)(F)F)O.NCC1CN(C1)C(=O)OC(C)(C)C.CCN(C(C)C)C(C)C.[N+](=O)([O-])C1=C(C=CC=C1)S(=O)(=O)Cl>>[N+](=O)([O-])C1=C(C=CC=C1)S(=O)(=O)N1CC(C1)CO
CC(C)(C)[O:17]C(=O)[N:13]1[CH2:14][CH:15]([CH2:16]N)[CH2:18]1.Cl[S:10]([c:9]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][cH:6][cH:7][cH:8]1)(=[O:11])=[O:12]>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[S:10](=[O:11])(=[O:12])[N:13]1[CH2:14][CH:15]([CH2:16][OH:17])[CH2:18]1
CC(C)(C)OC(=O)N1CC(CN)C1.O=[N+]([O-])c1ccccc1S(=O)(=O)Cl
O=[N+]([O-])c1ccccc1S(=O)(=O)N1CC(CO)C1
null
null
C(Cl)Cl
Acylation
OtherReaction
c9b078a4caf5c997901165af10960ed437a356b37bb74fff6be2fea2cd04573f
ebabfd3fff10853cf77efe5d8ae3f9cc562ad656b1c42b39d1bbf247c8359ebc
O=S(=O)(c1ccccc1)N1CCC1
C-C(-C)(-C)-[O;H0;D2;+0:1]-C(=O)-[N;H0;D3;+0:2]1-[C:3]-[C:4](-[CH2;D2;+0:5]-N)-[C:6]-1.Cl-[S;H0;D4;+0:7](=[O;D1;H0:8])(=[O;D1;H0:9])-[c:10](:[c:11]):[c:12]>>[O;D1;H0:8]=[S;H0;D4;+0:7](=[O;D1;H0:9])(-[N;H0;D3;+0:2]1-[C:3]-[C:4](-[CH2;D2;+0:5]-[OH;D1;+0:1])-[C:6]-1)-[c:10](:[c:11]):[c:12]
26
[{"value": 26.0, "product": "[N+](=O)([O-])C1=C(C=CC=C1)S(=O)(=O)N1CC(C1)CO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
17
HOUR
Tert-butyl 3-(aminomethyl)-1-azetidinecarboxylate (J. Med. Chem., (2001) 44:94-104) (441 mg, 2.35 mmol) was dissolved in CH2Cl2 (2 mL) and TFA (1.5 mL) and the mixture was stirred for 2 hours at room temperature. The volatiles were removed under reduced pressure and the residue was dissolved in dry MeOH (5 mL). Solid N...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Primary amine.Sulfonyl halide.Boc
Primary alcohol.Tertiary amine
C1C[NH]C1
C1C[NH]C1
c1ccccc1.C1C[NH]C1
HCl
C(Cl)Cl
null
17
CC(C)(C)OC(=O)N1CC(CN)C1.O=[N+]([O-])c1ccccc1S(=O)(=O)Cl>C(Cl)Cl>O=[N+]([O-])c1ccccc1S(=O)(=O)N1CC(CO)C1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-95b95e90c71f45ecbbe9619ba59fb7a4
Cc1cccnc1C1NC(c2ccccn2)CCC1C.O=[N+]([O-])c1ccccc1S(=O)(=O)N1CC(CO)C1>>Cc1cccnc1C1C(C)CCC(c2ccccn2)N1CC1CN(S(=O)(=O)c2ccccc2[N+](=O)[O-])C1
C(=O)(O)[O-].[Na+].[N+](=O)([O-])C1=C(C=CC=C1)S(=O)(=O)N1CC(C1)CO.CCN(CC)CC.CCN(C(C)C)C(C)C.CC=1C(=NC=CC1)C1NC(CCC1C)C1=NC=CC=C1.S(=O)(=O)(C)Cl>>CC=1C(=NC=CC1)C1N(C(CCC1C)C1=NC=CC=C1)CC1CN(C1)S(=O)(=O)C1=C(C=CC=C1)[N+](=O)[O-]
[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH:9]([CH3:10])[CH2:11][CH2:12][CH:13]([c:14]2[cH:15][cH:16][cH:17][cH:18][n:19]2)[NH:20]1.O[CH2:21][CH:22]1[CH2:23][N:24]([S:25](=[O:26])(=[O:27])[c:28]2[cH:29][cH:30][cH:31][cH:32][c:33]2[N+:34](=[O:35])[O-:36])[CH2:37]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:...
Cc1cccnc1C1NC(c2ccccn2)CCC1C.O=[N+]([O-])c1ccccc1S(=O)(=O)N1CC(CO)C1
Cc1cccnc1C1C(C)CCC(c2ccccn2)N1CC1CN(S(=O)(=O)c2ccccc2[N+](=O)[O-])C1
null
null
CCOC(=O)C
Functional Group Addition
OtherReaction
f03f6c9202affca8ab5230edf5678122ee5f9bfd569dea4217eba5e24f74f1c9
1019cc59ab0f350ad0daefd56a772ded1fa308745fe5d7f2116c2a78fd535d58
O=S(=O)(c1ccccc1)N1CC(CN2C(c3ccccn3)CCCC2c2ccccn2)C1
O-[CH2;D2;+0:1]-[C:2]1-[C:3]-[#7:4]-[C:5]-1.[#7;a:6]:[c:7]-[C:8](-[C:9])-[NH;D2;+0:10]-[C:11](-[c:12]:[#7;a:13])-[C:14]>>[#7;a:6]:[c:7]-[C:8](-[C:9])-[N;H0;D3;+0:10](-[CH2;D2;+0:1]-[C:2]1-[C:3]-[#7:4]-[C:5]-1)-[C:11](-[c:12]:[#7;a:13])-[C:14]
53.1
[{"value": 53.0, "product": "CC=1C(=NC=CC1)C1N(C(CCC1C)C1=NC=CC=C1)CC1CN(C1)S(=O)(=O)C1=C(C=CC=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 53.1, "product": "CC=1C(=NC=CC1)C1N(C(CCC1C)C1=NC=CC=C1)CC1CN(C1)S(=O)(=O)C1=C(C=CC=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desir...
null
null
1
HOUR
To a 0° C. solution of [1-(2-nitro-benzenesulfonyl)-azetidin-3-yl]-methanol (165 mg, 0.606 mmol) in EtOAc (15 mL) was added Et3N (0.101 mL, 0.727 mmol) then mesyl chloride (0.052 mL, 0.666 mmol). The reaction mixture was stirred for 1 hour at room temperature. The precipitate was filtered through a plug of Celite and w...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.C1C[NH]C1.c1ccccc1
HO-
CCOC(=O)C
null
1
Cc1cccnc1C1NC(c2ccccn2)CCC1C.O=[N+]([O-])c1ccccc1S(=O)(=O)N1CC(CO)C1>CCOC(=O)C>Cc1cccnc1C1C(C)CCC(c2ccccn2)N1CC1CN(S(=O)(=O)c2ccccc2[N+](=O)[O-])C1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-66f1a9641cb44e7daa1ddf8302288fe0
Cc1cccnc1C1C(C)CCC(c2ccccn2)N1CC1CN(S(=O)(=O)c2ccccc2[N+](=O)[O-])C1>>c1ccc(C2CCCC(c3ccccn3)N2CC2CNC2)nc1
CC=1C(=NC=CC1)C1N(C(CCC1C)C1=NC=CC=C1)CC1CN(C1)S(=O)(=O)C1=C(C=CC=C1)[N+](=O)[O-].C1(=CC=CC=C1)S.C(=O)([O-])[O-].[K+].[K+]>>N1CC(C1)CN1C(CCCC1C1=NC=CC=C1)C1=NC=CC=C1
C[c:3]1[cH:2][cH:1][cH:23][n:22][c:4]1[CH:5]1[CH:6](C)[CH2:7][CH2:8][CH:9]([c:10]2[cH:11][cH:12][cH:13][cH:14][n:15]2)[N:16]1[CH2:17][CH:18]1[CH2:19][N:20](S(=O)(=O)c2ccccc2[N+](=O)[O-])[CH2:21]1>>[cH:1]1[cH:2][cH:3][c:4]([CH:5]2[CH2:6][CH2:7][CH2:8][CH:9]([c:10]3[cH:11][cH:12][cH:13][cH:14][n:15]3)[N:16]2[CH2:17][CH:1...
Cc1cccnc1C1C(C)CCC(c2ccccn2)N1CC1CN(S(=O)(=O)c2ccccc2[N+](=O)[O-])C1
c1ccc(C2CCCC(c3ccccn3)N2CC2CNC2)nc1
null
null
CC#N
Reduction
OtherReaction
0bb4f82351d44fc53045df118d951e20c9995441f41cd68cf728d5a241ca8944
1e653e20ac001d92972e72ca6294e607303822683eea0adc1fa0a988ff7782b7
c1ccc(C2CCCC(c3ccccn3)N2CC2CNC2)nc1
C-[CH;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[#7:5](-[C:6]-[C:7]2-[C:8]-[N;H0;D3;+0:9](-S(=O)(=O)-c3:c:c:c:c:c:3-[N+](=O)-[O-])-[C:10]-2)-[C:11]-1-[c:12]1:[#7;a:13]:[c:14]:[c:15]:[c:16]:[c;H0;D3;+0:17]:1-C>>[#7;a:13]1:[c:14]:[c:15]:[c:16]:[cH;D2;+0:17]:[c:12]:1-[C:11]1-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]-[#7:5]-1-[C:6]-[C:7]1-[C:8]-[...
80
[{"value": 80.0, "product": "N1CC(C1)CN1C(CCCC1C1=NC=CC=C1)C1=NC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 74.5, "product": "N1CC(C1)CN1C(CCCC1C1=NC=CC=C1)C1=NC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
17
HOUR
A mixture of 3,3′-dimethyl-1′-[1-(2-nitro-benzenesulfonyl)-azetidin-3-ylmethyl]-1′,2′,3′4′,5′,6′-hexahydro-[2,2′;6′,2″]terpyridine (168 mg, 0.322 mmol), thiophenol (0.3 mL), K2CO3 (500 mg) in CH3CN (5 mL) were stirred at room temperature for 17 hours. The volatiles were removed under reduced pressure and saturated NaHC...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Tertiary amine
Secondary amine
c1ccncc1.C1CC[NH]CC1.C1C[NH]C1.c1ccccc1
c1ccncc1.C1CC[NH]CC1.C1CNC1
c1ccncc1.C1CC[NH]CC1.c1ccncc1.C1CNC1
HO-
CC#N
null
17
Cc1cccnc1C1C(C)CCC(c2ccccn2)N1CC1CN(S(=O)(=O)c2ccccc2[N+](=O)[O-])C1>CC#N>c1ccc(C2CCCC(c3ccccn3)N2CC2CNC2)nc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5c5da8fd01ab4a5194e715aeb5dde30c
CC(Br)C(C)Br.O=C1NC(=O)c2ccccc21>>O=C1c2ccccc2C(=O)N1CCCCBr
O.BrC(C(C)Br)C.C1(C=2C(C(N1)=O)=CC=CC2)=O.[K].CN(C=O)C>>BrCCCCN1C(C2=CC=CC=C2C1=O)=O
Br[CH:14]([CH3:13])[CH:15]([CH3:12])[Br:16].[O:1]=[C:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[C:9](=[O:10])[NH:11]1>>[O:1]=[C:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[C:9](=[O:10])[N:11]1[CH2:12][CH2:13][CH2:14][CH2:15][Br:16]
CC(Br)C(C)Br.O=C1NC(=O)c2ccccc21
O=C1c2ccccc2C(=O)N1CCCCBr
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
f628a96282a02c2d934b6182ac9e68df387900d55aea182cb7d0c7bf6035f5d2
3f4a0d64bf09050966e4d8460e04088119f0c5af483bc862484ff07ecabfc118
O=C1NC(=O)c2ccccc21
Br-[CH;D3;+0:1](-[CH3;D1;+0:2])-[CH;D3;+0:3](-[Br;D1;H0:4])-[CH3;D1;+0:5].[O;D1;H0:6]=[C:7]1-[NH;D2;+0:8]-[C:9](=[O;D1;H0:10])-[c:11]:[c:12]-1>>[Br;D1;H0:4]-[CH2;D2;+0:3]-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[CH2;D2;+0:5]-[N;H0;D3;+0:8]1-[C:9](=[O;D1;H0:10])-[c:11]:[c:12]-[C:7]-1=[O;D1;H0:6]
58
[{"value": 58.0, "product": "BrCCCCN1C(C2=CC=CC=C2C1=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
90
CELSIUS
5
HOUR
To a hot solution (90° C.) of dibromobutane (1.50 kg, 6.95 mol) in dimethylformamide (1.7 L) was added potassium phthalimide (329 g, 1.74 mol). The solution was stirred at 90° C. for 5 hours. The solution was cooled to room temperature prior to the addition of water (900 mL). The layers were separated and the aqueous l...
10.6084/m9.figshare.5104873.v1
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Secondary halide.Secondary halide.Unsubstituted dicarboximide
Primary halide.Substituted dicarboximide
c1ccc2c(c1)CNC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2
HBr
null
90
5
CC(Br)C(C)Br.O=C1NC(=O)c2ccccc21>>O=C1c2ccccc2C(=O)N1CCCCBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-16d3ff05724c49799b5dd239f1f80e7f
Cc1cccnc1C1CC(=O)CC(c2ncccc2C)N1>>Cc1cccnc1C1CCCC(c2ncccc2C)N1
CC=1C(=NC=CC1)C1NC(CC(C1)=O)C1=NC=CC=C1C.O.NN.[OH-].[K+]>>CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C
O=[C:10]1[CH2:9][CH:8]([c:7]2[c:2]([CH3:1])[cH:3][cH:4][cH:5][n:6]2)[NH:20][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[CH2:11]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][n:6][c:7]1[CH:8]1[CH2:9][CH2:10][CH2:11][CH:12]([c:13]2[n:14][cH:15][cH:16][cH:17][c:18]2[CH3:19])[NH:20]1
Cc1cccnc1C1CC(=O)CC(c2ncccc2C)N1
Cc1cccnc1C1CCCC(c2ncccc2C)N1
null
null
C(COCCO)O
Reduction
OtherReaction
480c86d699cecfc77c66c4f0456bd74413c6252cfa33cc10192db180010e8392
f9ba67182f94acd5fbe41487f8f71e26bccf898b8fc8091ef46f4363de5628d4
c1ccc(C2CCCC(c3ccccn3)N2)nc1
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1>>[#7:4]1-[C:3]-[C:2]-[CH2;D2;+0:1]-[C:6]-[C:5]-1
97
[{"value": 97.0, "product": "CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.7, "product": "CC=1C(=NC=CC1)C1NC(CCC1)C1=NC=CC=C1C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
125
CELSIUS
2
HOUR
To a solution of 3,3″-dimethyl-2′,3′,5′,6′-tetrahydro-1′H-[2,2′;6′,2″]terpyridin-4′-one (9.6 g, 34.1 mmol) in diethylene glycol (170 mL) was added hydrazine monohydrate (90 mL, 2.89 mol) and potassium hydroxide pellets (57.4 g, 1.02 mol) and the reaction stirred at 125° C. for 2 hours. 50 mL of hydrazine distilled off ...
10.6084/m9.figshare.5104873.v1
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Ketone
null
C1CCNCC1
C1CCNCC1
c1ccncc1.C1CCNCC1.c1ccncc1
Other
C(COCCO)O
125
2
Cc1cccnc1C1CC(=O)CC(c2ncccc2C)N1>C(COCCO)O>Cc1cccnc1C1CCCC(c2ncccc2C)N1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-4a15a491c355436d97368bb672ec079a
COC(=O)[C@@H](N)Cc1ccc(-c2ccccc2)cc1.Nc1ccc(Br)cc1C(=O)O>>COC(=O)[C@H](Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1N
COC([C@H](CC1=CC=C(C=C1)C1=CC=CC=C1)N)=O.BrC=1C=CC(=C(C(=O)O)C1)N>>COC([C@H](CC1=CC=C(C=C1)C1=CC=CC=C1)NC(C1=C(C=CC(=C1)Br)N)=O)=O
[CH3:1][O:2][C:3](=[O:4])[C@H:5]([CH2:6][c:7]1[cH:8][cH:9][c:10](-[c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[cH:17][cH:18]1)[NH2:19].O[C:20](=[O:21])[c:22]1[cH:23][c:24]([Br:25])[cH:26][cH:27][c:28]1[NH2:29]>>[CH3:1][O:2][C:3](=[O:4])[C@H:5]([CH2:6][c:7]1[cH:8][cH:9][c:10](-[c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2...
COC(=O)[C@@H](N)Cc1ccc(-c2ccccc2)cc1.Nc1ccc(Br)cc1C(=O)O
COC(=O)[C@H](Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1N
null
null
null
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(NCCc1ccc(-c2ccccc2)cc1)c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C:6]-[C:7](-[NH2;D1;+0:8])-[C:9](=[O;D1;H0:10])-[#8:11]-[C;D1;H3:12]>>[C:6]-[C:7](-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5])-[C:9](=[O;D1;H0:10])-[#8:11]-[C;D1;H3:12]
82.3
[{"value": 80.0, "product": "COC([C@H](CC1=CC=C(C=C1)C1=CC=CC=C1)NC(C1=C(C=CC(=C1)Br)N)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.3, "product": "COC([C@H](CC1=CC=C(C=C1)C1=CC=CC=C1)NC(C1=C(C=CC(=C1)Br)N)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
(2S)-(2-amino-5-bromo-benzoyl-amino)-3-biphenyl-4-yl-propionic acid methyl ester (1.53 g, 80%) was prepared from (2S)-amino-3-biphenyl-4-yl-propionic acid methyl ester (1.0 g, 4.1 mmol) and 5-bromo-2-amino-benzoic acid (1.23 g, 4.9 mmol) as described in procedure A. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
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Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HO-
null
null
null
COC(=O)[C@@H](N)Cc1ccc(-c2ccccc2)cc1.Nc1ccc(Br)cc1C(=O)O>>COC(=O)[C@H](Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1N
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ab00b5f3e45e4be3a73101d5ff61a76e
CC(C)(C)c1ccc(S(=O)(=O)Cl)cc1.COC(=O)[C@H](Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1N>>COC(=O)C(Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1NS(=O)(=O)c1ccc(C(C)(C)C)cc1
COC([C@H](CC1=CC=C(C=C1)C1=CC=CC=C1)NC(C1=C(C=CC(=C1)Br)N)=O)=O.N1=CC=CC=C1.C(C)(C)(C)C1=CC=C(C=C1)S(=O)(=O)Cl>>COC(C(CC1=CC=C(C=C1)C1=CC=CC=C1)NC(C1=C(C=CC(=C1)Br)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C)=O)=O
Cl[S:30](=[O:31])(=[O:32])[c:33]1[cH:34][cH:35][c:36]([C:37]([CH3:38])([CH3:39])[CH3:40])[cH:41][cH:42]1.[CH3:1][O:2][C:3](=[O:4])[C@H:5]([CH2:6][c:7]1[cH:8][cH:9][c:10](-[c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[cH:17][cH:18]1)[NH:19][C:20](=[O:21])[c:22]1[cH:23][c:24]([Br:25])[cH:26][cH:27][c:28]1[NH2:29]>>[CH3:1]...
CC(C)(C)c1ccc(S(=O)(=O)Cl)cc1.COC(=O)[C@H](Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1N
COC(=O)C(Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1NS(=O)(=O)c1ccc(C(C)(C)C)cc1
null
null
C(Cl)Cl
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
O=C(NCCc1ccc(-c2ccccc2)cc1)c1ccccc1NS(=O)(=O)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[#7:7]-[C:8](=[O;D1;H0:9])-[c:10]:[c:11](-[NH2;D1;+0:12]):[c:13]>>[#7:7]-[C:8](=[O;D1;H0:9])-[c:10]:[c:11](-[NH;D2;+0:12]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]):[c:13]
96.2
[{"value": 96.2, "product": "COC(C(CC1=CC=C(C=C1)C1=CC=CC=C1)NC(C1=C(C=CC(=C1)Br)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a stirring solution of (2S)-(2-amino-5-bromo-benzoyl-amino)-3-biphenyl-4-yl-propionic acid methyl ester (1.0 g, 2 mmol) prepared above dissolved in DCM containing pyridine (1.58 g, 4 mmol), was added 4-tert-butylbenzenesulfonyl chloride (1.20 g, 2.5 mmol) at 0° C. The reaction mixture was stirred at rt for 3 h, extr...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HCl
C(Cl)Cl
null
3
CC(C)(C)c1ccc(S(=O)(=O)Cl)cc1.COC(=O)[C@H](Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1N>C(Cl)Cl>COC(=O)C(Cc1ccc(-c2ccccc2)cc1)NC(=O)c1cc(Br)ccc1NS(=O)(=O)c1ccc(C(C)(C)C)cc1