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
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large_stringlengths
14
3.37k
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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-0387783899c642a8b7eb4ba379bcdf5d
ord-f83e86f633f84f5f9939b049f416c75f
COc1cc2nc(Cl)[nH]c(=O)c2cc1OC.Nc1ccncc1-c1cccc2c1CCNC2>>COc1cc2nc(N3CCc4c(cccc4-c4cnccc4N)C3)[nH]c(=O)c2cc1OC
ClC1=NC2=CC(=C(C=C2C(N1)=O)OC)OC.C1NCCC2=C(C=CC=C12)C=1C=NC=CC1N>>NC1=C(C=NC=C1)C1=C2CCN(CC2=CC=C1)C1=NC2=CC(=C(C=C2C(N1)=O)OC)OC
Cl[c:7]1[n:6][c:5]2[cH:4][c:3]([O:2][CH3:1])[c:30]([O:31][CH3:32])[cH:29][c:28]2[c:26](=[O:27])[nH:25]1.[NH:8]1[CH2:9][CH2:10][c:11]2[c:12]([cH:13][cH:14][cH:15][c:16]2-[c:17]2[cH:18][n:19][cH:20][cH:21][c:22]2[NH2:23])[CH2:24]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[n:6][c:7]([N:8]3[CH2:9][CH2:10][c:11]4[c:12]([cH:13][cH:14]...
COc1cc2nc(Cl)[nH]c(=O)c2cc1OC.Nc1ccncc1-c1cccc2c1CCNC2
COc1cc2nc(N3CCc4c(cccc4-c4cnccc4N)C3)[nH]c(=O)c2cc1OC
null
null
COC(C)O
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
1ff4e7e247e9c5784772ca9bff631974543ef5b92189117ec9f9de2907d7e038
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
O=c1[nH]c(N2CCc3c(cccc3-c3cccnc3)C2)nc2ccccc12
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[c:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5])-[C:9]-[c:10]
null
[]
95
CELSIUS
18
HOUR
A mixture of 2-chloro-6,7-dimethoxy-3H-quinazolin-4-one 1b (0.076 g, 0.31 mmol) and 3-(1,2,3,4-tetrahydro-isoquinolin-5-yl)-pyridin-4-ylamine (0.075 g, 0.33 mmol) in methoxyethanol (5 mL) was heated to 95° C. with stirring for 18 h the volatiles were evaporated and the residue was purified by flash column eluting with ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
c1ccc2ncncc2c1.c1ccc2c(c1)CCNC2
c1ccc2ncncc2c1.c1ccc2c(c1)CC[NH]C2
c1ccc2ncncc2c1.c1ccc2c(c1)CC[NH]C2.c1ccncc1
HCl
COC(C)O
95
18
COc1cc2nc(Cl)[nH]c(=O)c2cc1OC.Nc1ccncc1-c1cccc2c1CCNC2>COC(C)O>COc1cc2nc(N3CCc4c(cccc4-c4cnccc4N)C3)[nH]c(=O)c2cc1OC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-617f60e42998408eb2d6587c55676ac9
C1COCCN1.Clc1nccc2cnccc12>>c1cc2c(N3CCOCC3)nccc2cn1
ClC1=NC=CC2=CN=CC=C12.N1CCOCC1>>N1(CCOCC1)C1=NC=CC2=CN=CC=C12
[NH:5]1[CH2:6][CH2:7][O:8][CH2:9][CH2:10]1.Cl[c:4]1[c:3]2[cH:2][cH:1][n:16][cH:15][c:14]2[cH:13][cH:12][n:11]1>>[cH:1]1[cH:2][c:3]2[c:4]([N:5]3[CH2:6][CH2:7][O:8][CH2:9][CH2:10]3)[n:11][cH:12][cH:13][c:14]2[cH:15][n:16]1
C1COCCN1.Clc1nccc2cnccc12
c1cc2c(N3CCOCC3)nccc2cn1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
efb89a7fae314945df61cc249e6c54046a4ce960df3b95d10c9da0114efd0e05
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1cc2c(N3CCOCC3)nccc2cn1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[#8:10]1-[C:11]-[C:12]-[NH;D2;+0:13]-[C:14]-[C:15]-1>>[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:13]1-[C:14]-[C:15]-[#8:10]-[C:11]-[C:12]-1):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
null
[]
null
null
null
null
To 1-chloro-2,6-naphthyridine (164.3 mg, 0.998 mmol) (prepared as described in Van den Haak et al, J. Org. Chem 1982, 47 (9), 1673–7) was added morpholine (15 mL) and the mixture was heated at reflux for 4 h. Removal of the volatile components gave 216.6 mg of 1-morpholin-4-yl-[2,6]naphthyridine as a beige solid. Condi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1COCCN1.c1cc2cnccc2cn1
C1COCC[NH]1.c1cc2cnccc2cn1
C1COCC[NH]1.c1cc2cnccc2cn1
HCl
null
null
null
C1COCCN1.Clc1nccc2cnccc12>>c1cc2c(N3CCOCC3)nccc2cn1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6647c4f09b6c419a9d4dc6d55a619a4e
Brc1ccccc1.COc1cc2[nH]c(N3CCn4ccnc4C3)nc(=O)c2cc1OC.COc1cc2nc(Cl)[nH]c(=O)c2cc1OC>>COc1cc2[nH]c(N3CCn4c(-c5ccccc5)cnc4C3)nc(=O)c2cc1OC.[NH4+].[OH-]
BrC1=CC=CC=C1.ClC1=NC2=CC(=C(C=C2C(N1)=O)OC)OC.N=1C=CN2C1CN(CC2)C=2NC1=CC(=C(C=C1C(N2)=O)OC)OC.C([O-])([O-])=O.[K+].[K+].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.N=1C=CN2C1CNCC2>>[NH4+].[OH-].COC=1C=C2C(N=C(NC2=CC1OC)N1CC=2N(CC1)C(=CN2)C2=CC=CC=C2)=O
Br[c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1.[CH3:1][O:2][c:3]1[cH:4][c:5]2[nH:6][c:7]([N:8]3[CH2:9][CH2:10][n:11]4[cH:12][cH:19][n:20][c:21]4[CH2:22]3)[n:23][c:24](=[O:25])[c:26]2[cH:27][c:28]1[O:29][CH3:30].COc1cc2nc(Cl)[nH:31]c(=O)c2cc1OC>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[nH:6][c:7]([N:8]3[CH2:9][CH2:10][n:11]4[c:12]...
Brc1ccccc1.COc1cc2[nH]c(N3CCn4ccnc4C3)nc(=O)c2cc1OC.COc1cc2nc(Cl)[nH]c(=O)c2cc1OC
COc1cc2[nH]c(N3CCn4c(-c5ccccc5)cnc4C3)nc(=O)c2cc1OC.[NH4+].[OH-]
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
CN(C)C=O
C-C Coupling
OtherReaction
51f174b122b4148efe85294a56b64d149a95665eefd585d6934ae86691193038
96400e5d57c3fc3e239eb6559ef444ea690c3a427f5529d3d28176dd4529b3cf
O=c1nc(N2CCn3c(-c4ccccc4)cnc3C2)[nH]c2ccccc12
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].C-O-c1:c:c2:n:c(-Cl):[nH;D2;+0:6]:c(=O):c:2:c:c:1-O-C.[C:7]-[#7;a:8]1:[c:9]:[#7;a:10]:[c:11]:[cH;D2;+0:12]:1>>[C:7]-[#7;a:8]1:[c:9]:[#7;a:10]:[c:11]:[c;H0;D3;+0:12]:1-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[NH4+;D0:6]
null
[]
140
CELSIUS
null
null
5,6,7,8-Tetrahydro-imidazo[1,2-a]pyrazine, prepared as described in PCT Application WO 01/44250, was coupled with 2-chloro-6,7-dimethoxy-3H-quinazolin-4-one 1b, as described herein. 2-(5,6-dihydro-8H-imidazo[1,2-a]pyrazin-7-yl)-6,7-dimethoxy-1H-quinazolin-4-one (150 mg, 0.46 mmol) was combined with bromobezene (97 μL, ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Ether.Ether
null
c1ccccc1.c1cn2c(n1)C[NH]CC2.c1ccc2ncncc2c1
c1ccccc1.c1cn2c(n1)C[NH]CC2
c1ccc2ncncc2c1.c1ccccc1.c1cn2c(n1)C[NH]CC2
HCl.Br-
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].CN(C)C=O
140
null
Brc1ccccc1.COc1cc2[nH]c(N3CCn4ccnc4C3)nc(=O)c2cc1OC.COc1cc2nc(Cl)[nH]c(=O)c2cc1OC>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].CN(C)C=O>COc1cc2[nH]c(N3CCn4c(-c5ccccc5)cnc4C3)nc(=O)c2cc1OC.[NH4+].[OH-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4ba65496943c421e8ec262612b95b609
CCCCO.CP(=O)(Cl)Cl>>CCCCOP(C)(=O)O
C[C@@H]1CC[C@H]2C[C@@H](/C(=C/C=C/C=C/[C@H](C[C@H](C(=O)[C@@H]([C@@H](/C(=C/[C@H](C(=O)C[C@H](OC(=O)[C@@H]3CCCCN3C(=O)C(=O)[C@@]1(O2)O)[C@H](C)C[C@@H]4CC[C@H]([C@@H](C4)OC)O)C)/C)O)OC)C)C)/C)OC.C(=O)(O)[O-].[Na+].CP(=O)(Cl)Cl.N1=CC(=CC(=C1)C)C.N1=CC(=CC(=C1)C)C.C(CCC)O>>C(CCC)OP(O)(=O)C
[CH3:1][CH2:2][CH2:3][CH2:4][OH:5].Cl[P:6](Cl)([CH3:7])=[O:8]>>[CH3:1][CH2:2][CH2:3][CH2:4][O:5][P:6]([CH3:7])(=[O:8])[OH:9]
CCCCO.CP(=O)(Cl)Cl
CCCCOP(C)(=O)O
null
N1N=NN=C1
CCOC(=O)C.C(Cl)Cl
Functional Group Interconversion
OtherReaction
bbb792e2dbaac6137f4ab4b2ad2edf8b90c54de5f7db3b319a5444b78b4405dc
5700379a096deb40e2dc50b293f55a01cfe36aa58cf97bdfa006d0b7ff21038e
null
Cl-[P;H0;D4;+0:1](-Cl)(-[C;D1;H3:2])=[O;D1;H0:3].[C:4]-[C:5]-[OH;D1;+0:6]>>[C:4]-[C:5]-[O;H0;D2;+0:6]-[P;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])-[O;D1;H1:7]
376.5
[{"value": 376.5, "product": "C(CCC)OP(O)(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
8
HOUR
To a flask containing 1H-tetrazole (˜0.002 g, 0.028 mmol) was added a solution of n-butanol (0.041 g, 0.55 mmol) in 0.33 mL of DCM, followed by a solution of 3,5-lutidine (0.090 g, 0.84 mmol) in 0.33 mL of DCM. The resulting clear solution was cooled to 0° C. then added, under an atmosphere of N2, a solution of methylp...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
null
null
null
null
Other
N1N=NN=C1.CCOC(=O)C.C(Cl)Cl
0
8
CCCCO.CP(=O)(Cl)Cl>N1N=NN=C1.CCOC(=O)C.C(Cl)Cl>CCCCOP(C)(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6397b187f4af46799fe266abba7004ed
CC(=O)O[C@H]1C(=O)[C@@]2(C)[C@H]([C@H](OC(=O)c3ccccc3)[C@]3(O)C[C@H](OC(=O)[C@H](O)[C@@H](NC(=O)c4ccccc4)c4ccccc4)C(C)=C1C3(C)C)[C@]1(OC(C)=O)CO[C@@H]1C[C@@H]2O.CO[C@@]12[C@H](COC(N)=O)C3=C(C(=O)C(C)=C(N)C3=O)N1C[C@@H]1N[C@@H]12.COc1cccc2c1C(=O)c1c(O)c3c(c(O)c1C2=O)C[C@@](O)(C(=O)CO)C[C@@H]3O[C@H]1C[C@H](N)[C@H](O)[C@H...
CC1=C(C(=O)C2=C(C1=O)N3C[C@H]4[C@@H]([C@@]3([C@@H]2COC(=O)N)OC)N4)N.N(=NC(=O)OC(C)C)C(=O)OC(C)C.CC1=C2[C@H](C(=O)[C@@]3([C@H](C[C@@H]4[C@]([C@H]3[C@@H]([C@@](C2(C)C)(C[C@@H]1OC(=O)[C@@H]([C@H](C=5C=CC=CC5)NC(=O)C=6C=CC=CC6)O)O)OC(=O)C=7C=CC=CC7)(CO4)OC(=O)C)O)C)OC(=O)C.C[C@H]1[C@H]([C@H](C[C@@H](O1)O[C@H]2C[C@@](CC=3C2...
CC(=O)O[C@@]12CO[C@@H]1C[C@H](O)[C@@]1(C)C(=O)[C@H:16]([O:15]C(C)=O)C3=C(C)[C@@H](OC(=O)[C@H](O)[C@@H](NC(=O)[c:19]4ccccc4)c4ccccc4)C[C@@](O)([C@@H](OC(=O)c4ccccc4)[C@H]21)C3(C)C.C[C:7]1=[C:8](N)[C:9](=O)[C:4]2=[C:5](N3C[C@@H]4N[C@@H:21]4[C@:22]3([O:23]C)[C@@H:3]2COC(N)=O)[C:6]1=O.COc1cccc2c1C(=O)c1c(O)c3c(c(O)c1C2=O)C...
CC(=O)O[C@H]1C(=O)[C@@]2(C)[C@H]([C@H](OC(=O)c3ccccc3)[C@]3(O)C[C@H](OC(=O)[C@H](O)[C@@H](NC(=O)c4ccccc4)c4ccccc4)C(C)=C1C3(C)C)[C@]1(OC(C)=O)CO[C@@H]1C[C@@H]2O.CO[C@@]12[C@H](COC(N)=O)C3=C(C(=O)C(C)=C(N)C3=O)N1C[C@@H]1N[C@@H]12.COc1cccc2c1C(=O)c1c(O)c3c(c(O)c1C2=O)C[C@@](O)(C(=O)CO)C[C@@H]3O[C@H]1C[C@H](N)[C@H](O)[C@H...
COc1ccc(/C=C\c2cc(OC)c(OC)c(OC)c2)cc1O
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
a952d9c4cc02b540039f414cf22e48b597111dabf9a7e1389b29e740894644a1
98bcab2161137fee6bc0c4c66a26addfdcdd3e2f18092d3d98c96ef4b51f0aff
C(=C\c1ccccc1)\c1ccccc1
null
null
[]
null
null
null
null
Commercially available reagents and solvents were obtained as follows: HPLC-grade solvents, Fisher; anhydrous solvents, Aldrich; diisopropyl azodicarboxylate (DIAD, 95%), Lancaster; 4-aminobenzyl alcohol, Alfa Aesar; Z-val-OSu, Advanced ChemTech; L-citrulline, Novabiochem; (1S, 2R)-(+)-norephedrine and other commercial...
10.6084/m9.figshare.5104873.v1
null
Enamine.Enamine.Carbamic ester.Carboxylic acid.Ketone.Ketone.Ketone.Ketone.Ketone.Ketone.Ketone.Ketone.Ketone.Ester.Ester.Ester.Ester.Ether.Ether.Ether.Ether.Ether.Ether.Ether.Ether.Ether.Urea.Secondary amide.Primary alcohol.Primary alcohol.Primary alcohol.Secondary alcohol.Secondary alcohol.Secondary alcohol.Secondary...
Ether.Ether.Ether.Ether.Aromatic alcohol
C1=C2CC[C@@H]3CC[C@H]4OC[C@@H]4[C@H]3C[C@H](CC1)C2.c1ccccc1.c1ccccc1.c1ccccc1.C1=CCC2=C(C1)C[C@H]1[C@H]3N[C@H]3CN21.c1ccc2c(c1)Cc1cc3c(cc1C2)CCCC3.C1CCOCC1.C1CCOCC1.c1ccc2c(c1)Cc1cc3c(cc1C2)CCCC3.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
HO-
null
null
null
CC(=O)O[C@H]1C(=O)[C@@]2(C)[C@H]([C@H](OC(=O)c3ccccc3)[C@]3(O)C[C@H](OC(=O)[C@H](O)[C@@H](NC(=O)c4ccccc4)c4ccccc4)C(C)=C1C3(C)C)[C@]1(OC(C)=O)CO[C@@H]1C[C@@H]2O.CO[C@@]12[C@H](COC(N)=O)C3=C(C(=O)C(C)=C(N)C3=O)N1C[C@@H]1N[C@@H]12.COc1cccc2c1C(=O)c1c(O)c3c(c(O)c1C2=O)C[C@@](O)(C(=O)CO)C[C@@H]3O[C@H]1C[C@H](N)[C@H](O)[C@H...
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5062c37bf9ad4880a95eebcce007759c
CC(=O)O[BH-](OC(C)=O)OC(C)=O.CC(C)(C)OC(=O)C1(N)CCCC1>>CC(C)(C)OC(=O)C1(N)C=COC=C1
C(#N)[BH3-].[Na+].C(C)(C)(C)OC(=O)C1(CCCC1)N.C(C)(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+]>>C(C)(C)(C)OC(=O)C1(C=COC=C1)N
CC(=O)O[BH-](OC(C)=O)OC(C)=[O:12].C1[CH2:10][C:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])([NH2:9])[CH2:14][CH2:13]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C:8]1([NH2:9])[CH:10]=[CH:11][O:12][CH:13]=[CH:14]1
CC(=O)O[BH-](OC(C)=O)OC(C)=O.CC(C)(C)OC(=O)C1(N)CCCC1
CC(C)(C)OC(=O)C1(N)C=COC=C1
null
null
null
Acylation
OtherReaction
bd4e55b9a1806502487f17e5bc91d7ce55cfe35462a744004bb4316beb890800
94fdff9f10c6953a5a157a0a3d842c4d1e483ed489aa0d9d85a68c42c68923d0
C1=COC=CC1
C-C(=O)-O-[BH-](-O-C(-C)=O)-O-C(-C)=[O;H0;D1;+0:1].[C;D1;H3:2]-[C:3](-[C;D1;H3:4])(-[C;D1;H3:5])-[#8:6]-[C:7](=[O;D1;H0:8])-[C:9]1(-[N;D1;H2:10])-[CH2;D2;+0:11]-C-[CH2;D2;+0:12]-[CH2;D2;+0:13]-1>>[C;D1;H3:2]-[C:3](-[C;D1;H3:4])(-[C;D1;H3:5])-[#8:6]-[C:7](=[O;D1;H0:8])-[C:9]1(-[N;D1;H2:10])-[CH;D2;+0:11]=[C:14]-[O;H0;D2...
null
[]
null
null
null
null
An alternative route for the preparation of some 1,3,4-trisubstituted cyclopentanes within the scope of the instant invention is given in Scheme 11. Reductive alkylation, using for example sodium triacetoxyborohydride or sodium cyanoborohydride, of a cycloalkyl amino-acid 11-2, such as 1-aminocyclopentane carboxylic ac...
10.6084/m9.figshare.5104873.v1
null
null
Ether
C1CCCC1
C1=COC=CC1
C1=COC=CC1
HO-.B
null
null
null
CC(=O)O[BH-](OC(C)=O)OC(C)=O.CC(C)(C)OC(=O)C1(N)CCCC1>>CC(C)(C)OC(=O)C1(N)C=COC=C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b2d23674e1954e95b0862e72fba9eb4a
CC(C)(C)OC(=O)N1CCC(C(=O)O)CC1.C[Si](C)(C)C=[N+]=[N-]>>COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1
C(=O)(OC(C)(C)C)N1CCC(C(=O)O)CC1.C[Si](C)(C)C=[N+]=[N-]>>C(C)(C)(C)OC(=O)N1CCC(CC1)C(=O)OC
[OH:2][C:3](=[O:4])[CH:5]1[CH2:6][CH2:7][N:8]([C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15])[CH2:16][CH2:17]1.C[Si](C)(C)[CH:1]=[N+]=[N-]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:6][CH2:7][N:8]([C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15])[CH2:16][CH2:17]1
CC(C)(C)OC(=O)N1CCC(C(=O)O)CC1.C[Si](C)(C)C=[N+]=[N-]
COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1
null
null
ClCCl.CO
Heteroatom Alkylation and Arylation
O-alkylation of carboxylic acids with diazo compounds
39589be0e9a30df66714fe618d22a8ac0fb24901dbf2ead1ab33e31556c7ac64
8b539baf7aeb5ab868833e33306bad77200a853d562904197e13de2e27e229d7
C1CCNCC1
C-[Si](-C)(-C)-[CH;D2;+0:1]=[N+]=[N-].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
96.6
[{"value": 96.6, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of BOC-isonipecotic acid (45.0 g, 0.20 mol) dissolved in a 3:1 solution of dichloromethane/methanol (1200 mL) at 0° C. was added a solution of trimethylsilyldiazomethane (147 mL, 0.29 mol, 2.0M in hexane) over 30 min via an addition funnel. The reaction mixture was then concentrated to afford the title co...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Diazo.Silyl protective group
Ester
null
null
C1CC[NH]CC1
Other
ClCCl.CO
null
null
CC(C)(C)OC(=O)N1CCC(C(=O)O)CC1.C[Si](C)(C)C=[N+]=[N-]>ClCCl.CO>COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-292d55b0aa854c219dbd269febe9a838
C=CCCCBr.COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1>>C=CCCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1
C([O-])(O)=O.[Na+].C[Si](C)(C)[N-][Si](C)(C)C.[K+].C(C)(C)(C)OC(=O)N1CCC(CC1)C(=O)OC.BrCCCC=C>>C(CCC=C)C1(CCN(CC1)C(=O)OC(C)(C)C)C(=O)OC
Br[CH2:5][CH2:4][CH2:3][CH:2]=[CH2:1].[CH:6]1([C:7](=[O:8])[O:9][CH3:10])[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:21][CH2:22]1>>[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][C:6]1([C:7](=[O:8])[O:9][CH3:10])[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[...
C=CCCCBr.COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1
C=CCCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1
null
null
O1CCCC1
C-C Coupling
OtherReaction
cc17dfd0def644ca87e815e637357310f207eb90d8b3273b51858e3602d79eca
0061a06af9fc64155952582b91b574e4abd8908ca14244f15179c2400b24dd08
C1CCNCC1
Br-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]=[C;D1;H2:5].[C;D1;H3:6]-[#8:7]-[C:8](=[O;D1;H0:9])-[CH;D3;+0:10]1-[C:11]-[C:12]-[#7:13]-[C:14]-[C:15]-1>>[C;D1;H2:5]=[C:4]-[C:3]-[C:2]-[CH2;D2;+0:1]-[C;H0;D4;+0:10]1(-[C:8](=[O;D1;H0:9])-[#8:7]-[C;D1;H3:6])-[C:11]-[C:12]-[#7:13]-[C:14]-[C:15]-1
99.2
[{"value": 99.2, "product": "C(CCC=C)C1(CCN(CC1)C(=O)OC(C)(C)C)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of potassium bis(trimethylsilyl)amide (30.7 g, 0.15 mol) in tetrahydrofuran (750 mL) at 0° C. was added a solution of methyl 1-(tert-butoxycarbonyl)piperidine-4-carboxylate (25 g, 0.10 mol) from Step A in tetrahydrofuran (250 mL) and the reaction mixture was stirred for 1 h. 5-Bromo-1-pentene (19.4 mL, 0....
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester
Ester
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1
HBr
O1CCCC1
null
1
C=CCCCBr.COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1>O1CCCC1>C=CCCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-093ff50ed82045c98be5e1147b0de0d3
C=CCCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1.CO>>COC(=O)C1(CCCC=O)CCN(C(=O)OC(C)(C)C)CC1
C(CCC=C)C1(CCN(CC1)C(=O)OC(C)(C)C)C(=O)OC.CO.CSC>>O=CCCCC1(CCN(CC1)C(=O)OC(C)(C)C)C(=O)OC
C=[CH:9][CH2:8][CH2:7][CH2:6][C:5]1([C:3]([O:2][CH3:1])=[O:4])[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:21][CH2:22]1.C[OH:10]>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][CH2:7][CH2:8][CH:9]=[O:10])[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:...
C=CCCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1.CO
COC(=O)C1(CCCC=O)CCN(C(=O)OC(C)(C)C)CC1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
819cc56f1de0795ade47bb88544c1667e77ababe1a9f8886b0ab43d7fc61baf3
d60fee5fdd239063d17d89701ffcf20659b907d096a729f7ffeb7d37370ddb04
C1CCNCC1
C-[OH;D1;+0:1].C=[CH;D2;+0:2]-[C:3]-[C:4]>>[C:4]-[C:3]-[CH;D2;+0:2]=[O;H0;D1;+0:1]
null
[]
null
null
null
null
A solution of methyl 4-(pent-4-en-1-yl)-1-(tert-butoxycarbonyl)piperidine-4-carboxylate (29.4 g, 0.0945 mol) from Step B in methanol (1000 mL) was cooled to −78° C. in a dry ice/methanol bath and ozone was bubbled into the solution until a blue color persisted. The excess ozone was removed with a stream of nitrogen and...
10.6084/m9.figshare.5104873.v1
null
Allyl.Methanol
Aldehyde
null
null
C1CC[NH]CC1
Other
null
null
null
C=CCCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1.CO>>COC(=O)C1(CCCC=O)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-190dcd50c65c412eb9c6458f3623a7b2
COC(=O)C1(CCCC=O)CCN(C(=O)OC(C)(C)C)CC1>>COC(=O)C1(CCCC(=O)O)CCN(C(=O)OC(C)(C)C)CC1
O=CCCCC1(CCN(CC1)C(=O)OC(C)(C)C)C(=O)OC.CC(=O)C.OS(=O)(=O)O.O=[Cr](=O)=O>>C(C)(C)(C)OC(=O)N1CCC(CC1)(C(=O)OC)CCCC(=O)O
[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][CH2:7][CH2:8][CH:9]=[O:10])[CH2:12][CH2:13][N:14]([C:15](=[O:16])[O:17][C:18]([CH3:19])([CH3:20])[CH3:21])[CH2:22][CH2:23]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][CH2:7][CH2:8][C:9](=[O:10])[OH:11])[CH2:12][CH2:13][N:14]([C:15](=[O:16])[O:17][C:18]([CH3:19])([CH3:20])[CH3:21])[...
COC(=O)C1(CCCC=O)CCN(C(=O)OC(C)(C)C)CC1
COC(=O)C1(CCCC(=O)O)CCN(C(=O)OC(C)(C)C)CC1
null
null
CC(=O)C
Oxidation
Oxidation of aldehydes to carboxylic acids
53d556378d4cb30c33d50a2e1886f8fba4abcbb7065d1faceeb5e5968b58008d
2f35b69536247c389825da7241226b4e568110d1cfe736c83136d58ad1c9dae2
C1CCNCC1
[C:1]-[C:2]-[CH;D2;+0:3]=[O;D1;H0:4]>>[C:1]-[C:2]-[C;H0;D3;+0:3](=[O;D1;H0:4])-[O;D1;H1:5]
null
[]
null
null
5
MINUTE
To a solution of methyl 4-(4-oxobut-1-yl)-1-(tert-butoxycarbonyl)piperidine-4-carboxylate (23.0 g, 0.0734 mol) from Step C in acetone (775 mL) at room temperature was added Jones reagent (28.2 mL, 2.6M) via syringe. After 5 min, the reaction mixture was concentrated. The residue was taken up in water and diethyl ether ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Carboxylic acid
null
null
C1CC[NH]CC1
Other
CC(=O)C
null
0.083333
COC(=O)C1(CCCC=O)CCN(C(=O)OC(C)(C)C)CC1>CC(=O)C>COC(=O)C1(CCCC(=O)O)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6b2aefe82fc74fb8a87e403b637a98cc
COC(=O)C1(CCCC(=O)O)CCN(C(=O)OC(C)(C)C)CC1.C[Si](C)(C)C=[N+]=[N-]>>COC(=O)CCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1
C(C)(C)(C)OC(=O)N1CCC(CC1)(C(=O)OC)CCCC(=O)O.C[Si](C)(C)C=[N+]=[N-]>>C(C)(C)(C)OC(=O)N1CCC(CC1)(C(=O)OC)CCCC(=O)OC
[OH:2][C:3](=[O:4])[CH2:5][CH2:6][CH2:7][C:8]1([C:9](=[O:10])[O:11][CH3:12])[CH2:13][CH2:14][N:15]([C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])[CH2:23][CH2:24]1.C[Si](C)(C)[CH:1]=[N+]=[N-]>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][CH2:6][CH2:7][C:8]1([C:9](=[O:10])[O:11][CH3:12])[CH2:13][CH2:14][N:15]([C:16](=[O:17...
COC(=O)C1(CCCC(=O)O)CCN(C(=O)OC(C)(C)C)CC1.C[Si](C)(C)C=[N+]=[N-]
COC(=O)CCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1
null
null
ClCCl.CO
Heteroatom Alkylation and Arylation
O-alkylation of carboxylic acids with diazo compounds
39589be0e9a30df66714fe618d22a8ac0fb24901dbf2ead1ab33e31556c7ac64
8b539baf7aeb5ab868833e33306bad77200a853d562904197e13de2e27e229d7
C1CCNCC1
C-[Si](-C)(-C)-[CH;D2;+0:1]=[N+]=[N-].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
82.4
[{"value": 82.4, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)(C(=O)OC)CCCC(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To a solution of 4-(1-(tert-butoxycarbonyl)-4-(methoxy-carbonyl)piperidin-4-yl)butanoic acid (23.4 g, 0.071 mol) from Step D in 3:1 dichloromethane/methanol (480 mL) at 0° C. was added a solution of trimethylsilyldiazomethane (53 mL, 0.11 mol, 2.0M in hexane). The reaction mixture was stirred for 15 min and then concen...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Diazo.Silyl protective group
Ester
null
null
C1CC[NH]CC1
Other
ClCCl.CO
null
0.25
COC(=O)C1(CCCC(=O)O)CCN(C(=O)OC(C)(C)C)CC1.C[Si](C)(C)C=[N+]=[N-]>ClCCl.CO>COC(=O)CCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2199290325e045e6997c103221fdd023
COC(=O)CCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1>>COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
O1CCCC1.C(C)(C)[N-]C(C)C.[Li+].C(C)(C)(C)OC(=O)N1CCC(CC1)(C(=O)OC)CCCC(=O)OC.O1CCCC1.C(C)(C)[N-]C(C)C.[Li+].[Cl-].[NH4+].C(C)(=O)OCC>>COC(=O)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O
CO[C:21]([C:8]1([CH2:7][CH2:6][CH2:5][C:3]([O:2][CH3:1])=[O:4])[CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]1)=[O:22]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:6][CH2:7][C:8]2([CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]2)[C:...
COC(=O)CCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1
COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
null
null
O1CCCC1
Functional Group Interconversion
OtherReaction
fdbcf46d25defdaa148ed0cf50374ec5c2675fb6f93e6d5b812ee842c73dfa8d
6f130a746a78d10ca37f94948711de2b0c76f45052ca887b0e681c66276a7764
O=C1CCCC12CCNCC2
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4]-[C:5]-[CH2;D2;+0:6]-[C:7](=[O;D1;H0:8])-[#8:9]-[C;D1;H3:10])(-[C:11])-[C:12]>>[C:11]-[C:3]1(-[C:12])-[C:4]-[C:5]-[CH;D3;+0:6](-[C:7](=[O;D1;H0:8])-[#8:9]-[C;D1;H3:10])-[C;H0;D3;+0:1]-1=[O;D1;H0:2]
110.2
[{"value": 110.2, "product": "COC(=O)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
25
MINUTE
To a solution of methyl 4-(1-(tert-butoxycarbonyl)-4-(methoxycarbonyl)piperidin-4-yl)butanoate (20.1 g, 0.058 mol) from Step E in tetrahydrofuran (600 mL) at −78° C. was added lithium diisopropylamide mono(tetrahydrofuran) (47 mL, 0.070 mol, 1.5M solution in cyclohexanes). The reaction mixture was stirred at −78° C. fo...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Ketone
null
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
HO-
O1CCCC1
-78
0.416667
COC(=O)CCCC1(C(=O)OC)CCN(C(=O)OC(C)(C)C)CC1>O1CCCC1>COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-279bb325608143949a9c5045f8750794
COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O>>CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1
COC(=O)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O.[OH-].[Li+]>>O=C1CCCC12CCN(CC2)C(=O)OC(C)(C)C
COC(=O)[CH:14]1[CH2:13][CH2:12][C:11]2([CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:18][CH2:17]2)[C:15]1=[O:16]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]2([CH2:12][CH2:13][CH2:14][C:15]2=[O:16])[CH2:17][CH2:18]1
COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1
null
null
C(C)O.O1CCCC1.O
Reduction
Decarboxylation
2a633e18f5bcad5f2ae1e8675360a573985c0816d41c2f33a88053978877ccf7
f277909394d9f4e61cc2cdb65fef123102672ca91cfff7f8513cb0baf66138ac
O=C1CCCC12CCNCC2
C-O-C(=O)-[CH;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1=[O;D1;H0:6]>>[O;D1;H0:6]=[C:5]1-[C:4]-[C:3]-[C:2]-[CH2;D2;+0:1]-1
67.5
[{"value": 67.5, "product": "O=C1CCCC12CCN(CC2)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
90
CELSIUS
null
null
To a solution of tert-butyl 2-(methoxycarbonyl)-1-oxo-8-azaspiro[4.5]decane-8-carboxylate (17.2 g, 0.055 mol) from Step F in a 2:2:1 mixture of ethanol/tetrahydrofuran/water (555 mL) was added pulverized lithium hydroxide (26 g, 1.10 mol). The reaction mixture was heated to 90° C. for 60 h. The reaction mixture was all...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester
Ketone
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
HO-
C(C)O.O1CCCC1.O
90
null
COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O>C(C)O.O1CCCC1.O>CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f4d34c0f487347f9a801ff3387bd1e3d
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CCC=O>>CCC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
[Cl-].[NH4+].O=C1CCCC12CCN(CC2)C(=O)OC(C)(C)C.O1CCCC1.C(C)(C)[N-]C(C)C.[Li+].C(CC)=O>>OC(CC)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O
[CH2:5]1[CH2:6][CH2:7][C:8]2([CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]2)[C:21]1=[O:22].[CH3:1][CH2:2][CH:3]=[O:4]>>[CH3:1][CH2:2][CH:3]([OH:4])[CH:5]1[CH2:6][CH2:7][C:8]2([CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]2)...
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CCC=O
CCC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
null
null
C(C)OCC
C-C Coupling
OtherReaction
0608dea009714d2fb6fc79421f83631a68b8a53e44927021afcf353589bd65c5
7d7139092067ff475e8e8a4ad6adb4833600ca969e282ed08dc56c016dccb864
O=C1CCCC12CCNCC2
[C;D1;H3:1]-[C:2]-[CH;D2;+0:3]=[O;H0;D1;+0:4].[O;D1;H0:5]=[C:6]1-[C:7]-[C:8]-[C:9]-[CH2;D2;+0:10]-1>>[C;D1;H3:1]-[C:2]-[CH;D3;+0:3](-[OH;D1;+0:4])-[CH;D3;+0:10]1-[C:9]-[C:8]-[C:7]-[C:6]-1=[O;D1;H0:5]
120.9
[{"value": 120.9, "product": "OC(CC)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
30
MINUTE
tert-Butyl 1-oxo-8-azaspiro[4.5]decane-8-carboxylate from Step G (4.5 g, 17.8 mmol) was dried by evaporating with toluene (10 mL) three times in vacuo, dissolved in tetrahydrofuran (100 mL), and cooled to −78° C. To this solution was added lithium diisopropylamide mono(tetrahydrofuran) (24 mL, 36 mmol, 1.5 M in cyclohe...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone.Secondary alcohol
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
null
C(C)OCC
-78
0.5
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CCC=O>C(C)OCC>CCC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c0879ba6ad3742769d2b05b03691ff97
CCC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O>>CCC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
C(C)N(CC)CC.C(C(=O)Cl)(=O)Cl.CS(=O)C.OC(CC)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O>>O=C(CC)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O
[CH3:1][CH2:2][CH:3]([OH:4])[CH:5]1[CH2:6][CH2:7][C:8]2([CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]2)[C:21]1=[O:22]>>[CH3:1][CH2:2][C:3](=[O:4])[CH:5]1[CH2:6][CH2:7][C:8]2([CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]2)[...
CCC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
CCC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
null
null
ClCCl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
c7c20d2959ac48847b03cc1265962cf99a8ec8a85900c087dabb30077298c66c
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
O=C1CCCC12CCNCC2
[C:1]-[C:2](-[CH;D3;+0:3](-[OH;D1;+0:4])-[C:5]-[C;D1;H3:6])-[C:7](=[O;D1;H0:8])-[C:9]>>[C:1]-[C:2](-[C;H0;D3;+0:3](=[O;H0;D1;+0:4])-[C:5]-[C;D1;H3:6])-[C:7](=[O;D1;H0:8])-[C:9]
84.1
[{"value": 84.1, "product": "O=C(CC)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
5
MINUTE
To a solution of oxalyl chloride (1.6 mL, 18.3 mmol) in dichloromethane (150 mL) at −78° C. was slowly added dimethyl sulfoxide (2.6 mL, 37 mmol). After 5 min, a solution of tert-butyl 2-(1-hydroxyprop-1-yl)-1-oxo-8-azaspiro[4.5]decane-8-carboxylate (4.75 g, 15.3 mmol) from Step H in dichloromethane (40 mL) was added v...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
null
null
C1CCC2(C1)CC[NH]CC2
null
ClCCl
-78
0.083333
CCC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O>ClCCl>CCC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0c06c86d3f3444378259f57ae88f4d91
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CC=O>>CC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
[Cl-].[NH4+].O=C1CCCC12CCN(CC2)C(=O)OC(C)(C)C.O1CCCC1.C(C)(C)[N-]C(C)C.[Li+].C(C)=O>>OC(C)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O
[CH2:4]1[CH2:5][CH2:6][C:7]2([CH2:8][CH2:9][N:10]([C:11](=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[CH3:17])[CH2:18][CH2:19]2)[C:20]1=[O:21].[CH3:1][CH:2]=[O:3]>>[CH3:1][CH:2]([OH:3])[CH:4]1[CH2:5][CH2:6][C:7]2([CH2:8][CH2:9][N:10]([C:11](=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[CH3:17])[CH2:18][CH2:19]2)[C:20]1=[O:21]
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CC=O
CC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
null
null
C(C)OCC
C-C Coupling
OtherReaction
0608dea009714d2fb6fc79421f83631a68b8a53e44927021afcf353589bd65c5
7d7139092067ff475e8e8a4ad6adb4833600ca969e282ed08dc56c016dccb864
O=C1CCCC12CCNCC2
[C;D1;H3:1]-[CH;D2;+0:2]=[O;H0;D1;+0:3].[O;D1;H0:4]=[C:5]1-[C:6]-[C:7]-[C:8]-[CH2;D2;+0:9]-1>>[C;D1;H3:1]-[CH;D3;+0:2](-[OH;D1;+0:3])-[CH;D3;+0:9]1-[C:8]-[C:7]-[C:6]-[C:5]-1=[O;D1;H0:4]
479.3
[{"value": 479.3, "product": "OC(C)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
35
MINUTE
tert-Butyl 1-oxo-8-azaspiro[4.5]decane-8-carboxylate from Procedure 1, Step G (1.2 g, 4.70 mmol) was dried by evaporating with toluene (5 mL) three times in vacuo, dissolved in tetrahydrofuran (50 mL), and cooled to −78° C. To this solution was added lithium diisopropylamide mono(tetrahydrofuran) (6.3 mL, 9.4 mmol, 1.5...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone.Secondary alcohol
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
null
C(C)OCC
-78
0.583333
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CC=O>C(C)OCC>CC(O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-01aabc2e796f428ba758c5068521a6d6
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CCOC=O>>CC(C)(C)OC(=O)N1CCC2(CCC(CO)C2=O)CC1
Cl.O=C1CCCC12CCN(CC2)C(=O)OC(C)(C)C.C(=O)OCC.CC(C)([O-])C.[K+]>>OCC1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]2([CH2:12][CH2:13][CH2:14][C:17]2=[O:18])[CH2:19][CH2:20]1.CCO[CH:15]=[O:16]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]2([CH2:12][CH2:13][CH:14]([CH2:15][OH:16])[C:17]2=[O:18])[CH2:19][CH2:20]1
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CCOC=O
CC(C)(C)OC(=O)N1CCC2(CCC(CO)C2=O)CC1
null
null
C(C)OCC
C-C Coupling
OtherReaction
ffec183098c03479e4a94391acf17db5e4f037a4dd9bf7d5e807c1809ed885c2
5190634190ddef4dc4ac4507891dca9c66c26991d95954d4514241a45c93ba26
O=C1CCCC12CCNCC2
C-C-O-[CH;D2;+0:1]=[O;H0;D1;+0:2].[O;D1;H0:3]=[C:4]1-[C:5]-[C:6]-[C:7]-[CH2;D2;+0:8]-1>>[O;D1;H0:3]=[C:4]1-[C:5]-[C:6]-[C:7]-[CH;D3;+0:8]-1-[CH2;D2;+0:1]-[OH;D1;+0:2]
51.4
[{"value": 51.4, "product": "OCC1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
2
DAY
tert-Butyl 1-oxo-8-azaspiro[4.5]decane-8-carboxylate from Procedure 1, Step G (0.526 g, 2.08 mmol) was dried by evaporating with toluene (10 mL) three times in vacuo, dissolved in methyl-tert-butyl ether (5 mL), and cooled to −78° C. To this solution was added ethyl formate (0.336 mL, 4.15 mmol) and then potassium t-bu...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ether
Ketone.Primary alcohol
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
HO-
C(C)OCC
-78
48
CC(C)(C)OC(=O)N1CCC2(CCCC2=O)CC1.CCOC=O>C(C)OCC>CC(C)(C)OC(=O)N1CCC2(CCC(CO)C2=O)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-701f21b2c1d643e889f13cae87e55dcf
COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O.NN>>CC(C)(C)OC(=O)N1CCC2(CCc3c2[nH][nH]c3=O)CC1
COC(=O)C1C(C2(CC1)CCN(CC2)C(=O)OC(C)(C)C)=O.NN>>C(C)(C)(C)OC(=O)N1CCC2(CC1)CCC=1C(NNC12)=O
CO[C:18]([CH:14]1[CH2:13][CH2:12][C:11]2([CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:21][CH2:20]2)[C:15]1=O)=[O:19].[NH2:16][NH2:17]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]2([CH2:12][CH2:13][c:14]3[c:15]2[nH:16][nH:17][c:18]3=[O:19])[CH2:20][CH2:21]1
COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O.NN
CC(C)(C)OC(=O)N1CCC2(CCc3c2[nH][nH]c3=O)CC1
null
null
C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
b2393f5ac303949ae2f8c96993959cb5eae8c5a8c32c1d0f6b02ba97ef7f919b
f32fac81dfdb000dc8678b0df4fe3b0a64c38caab136205f41649f692b09b3bd
O=c1[nH][nH]c2c1CCC21CCNCC1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH;D3;+0:3]1-[C:4]-[C:5]-[C:6](-[C:7])(-[C:8])-[C;H0;D3;+0:9]-1=O.[NH2;D1;+0:10]-[NH2;D1;+0:11]>>[C:7]-[C:6]1(-[C:8])-[C:5]-[C:4]-[c;H0;D3;+0:3]2:[c;H0;D3;+0:9]-1:[nH;D2;+0:10]:[nH;D2;+0:11]:[c;H0;D3;+0:1]:2=[O;D1;H0:2]
61.4
[{"value": 61.4, "product": "C(C)(C)(C)OC(=O)N1CCC2(CC1)CCC=1C(NNC12)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of tert-butyl 2-(methoxycarbonyl)-1-oxo-8-azaspiro[4.5]decane-8-carboxate from Procedure 1, Step F (0.448 g, 1.46 mmol) in toluene (15 mL) was added hydrazine (0.084 mL, 1.72 mmol). The reaction mixture was refluxed for 12 h, concentrated and the residue was purified by flash chromatography eluting with 5...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ester
null
C1CCC2(C1)CC[NH]CC2
c1nnc2c1CCC21CCNCC1
c1nnc2c1CCC21CCNCC1
HO-
C1(=CC=CC=C1)C
null
null
COC(=O)C1CCC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O.NN>C1(=CC=CC=C1)C>CC(C)(C)OC(=O)N1CCC2(CCc3c2[nH][nH]c3=O)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-51623ca6fed2402986932fa772644519
COC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1>>COC1(C(C)=O)CCN(C(=O)OC(C)(C)C)CC1
[F-].C(CCC)[N+](CCCC)(CCCC)CCCC.C[Si](C)(C)C[Li].[Cl-].[NH4+].C[Si](C)(C)C[Li].COC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)OC>>C(C)(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)OC
O([C:4]([C:3]1([O:2][CH3:1])[CH2:7][CH2:8][N:9]([C:10](=[O:11])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16])[CH2:17][CH2:18]1)=[O:6])[CH3:5]>>[CH3:1][O:2][C:3]1([C:4]([CH3:5])=[O:6])[CH2:7][CH2:8][N:9]([C:10](=[O:11])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16])[CH2:17][CH2:18]1
COC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
COC1(C(C)=O)CCN(C(=O)OC(C)(C)C)CC1
null
null
C(C)(=O)OCC.O.O1CCCC1.C(C)OCC
Miscellaneous
OtherReaction
3724e934ace06da3205b28d40bd9eba0c9f8214e3431e58c6de85eacba50eaae
0ffdc15c7ac34be51edf4589ed8aa3f210774f50305a479999afbf21400d0a96
C1CCNCC1
[#8:1]-[C:2](-[C;H0;D3;+0:3](=[O;D1;H0:4])-O-[CH3;D1;+0:5])(-[C:6])-[C:7]>>[#8:1]-[C:2](-[C;H0;D3;+0:3](-[CH3;D1;+0:5])=[O;D1;H0:4])(-[C:6])-[C:7]
37.1
[{"value": 37.1, "product": "C(C)(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 1-tert-butyl 4-methoxycarbonyl-4-methoxypiperidine-1-carboxylate (2.5 g, 9.05 mmol) dissolved in 100 mL of tetrahydrofuran at −78° C. was added trimethylsilylmethyl lithium (23 mL, 23 mmol). After 30 min additional trimethylsilylmethyl lithium (2.7 mL, 2.7 mmol) was added. The reaction mixture was then...
10.6084/m9.figshare.5104873.v1
null
Ester
Ketone
null
null
C1CC[NH]CC1
Other
C(C)(=O)OCC.O.O1CCCC1.C(C)OCC
null
0.5
COC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1>C(C)(=O)OCC.O.O1CCCC1.C(C)OCC>COC1(C(C)=O)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b89820f3efd14138aa3a6cb136df92cc
CCC=O.COC1(C(C)=O)CCN(C(=O)OC(C)(C)C)CC1>>CCC(O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
[Cl-].[NH4+].C(CC)=O.C(C)(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)OC.C(C)(C)NC(C)C.[Li]>>OC(CC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)OC)CC
[CH3:1][CH2:2][CH:3]=[O:4].[CH3:5][C:6](=[O:7])[C:8]1([O:9][CH3:10])[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:21][CH2:22]1>>[CH3:1][CH2:2][CH:3]([OH:4])[CH2:5][C:6](=[O:7])[C:8]1([O:9][CH3:10])[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:2...
CCC=O.COC1(C(C)=O)CCN(C(=O)OC(C)(C)C)CC1
CCC(O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
null
null
O1CCCC1
C-C Coupling
OtherReaction
d08eb7b2615717189cce315501bb2cfa7ee3668e6d8eaa24218b092d1454a850
7d7139092067ff475e8e8a4ad6adb4833600ca969e282ed08dc56c016dccb864
C1CCNCC1
[C;D1;H3:1]-[C:2]-[CH;D2;+0:3]=[O;H0;D1;+0:4].[C:5]-[C:6](-[CH3;D1;+0:7])=[O;D1;H0:8]>>[C:5]-[C:6](=[O;D1;H0:8])-[CH2;D2;+0:7]-[CH;D3;+0:3](-[OH;D1;+0:4])-[C:2]-[C;D1;H3:1]
55.9
[{"value": 55.9, "product": "OC(CC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)OC)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
To a solution of tert-butyl 4-acetyl-4-methoxypiperidine-1-carboxylate (0.589 g, 2.29 mmol) from Step A in tetrahydrofuran (20 mL) at −78° C. was added lithium diisopropylamine (0.650 mL, 0.974 mmol) followed by propionaldehyde (0.266 g, 0.330 mL, 4.58 mmol). After 5 min, the reaction mixture was poured into saturated ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone.Secondary alcohol
null
null
C1CC[NH]CC1
null
O1CCCC1
null
0.083333
CCC=O.COC1(C(C)=O)CCN(C(=O)OC(C)(C)C)CC1>O1CCCC1>CCC(O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2abda1273cd6457e8d73afd6e5bd1098
CCC(O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1>>CCC(=O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
C(C)N(CC)CC.C(C(=O)Cl)(=O)Cl.CS(=O)C.OC(CC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)OC)CC>>COC1(CCN(CC1)C(=O)OC(C)(C)C)C(CC(CC)=O)=O
[CH3:1][CH2:2][CH:3]([OH:4])[CH2:5][C:6](=[O:7])[C:8]1([O:9][CH3:10])[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:21][CH2:22]1>>[CH3:1][CH2:2][C:3](=[O:4])[CH2:5][C:6](=[O:7])[C:8]1([O:9][CH3:10])[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:2...
CCC(O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
CCC(=O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
null
null
ClCCl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
c7c20d2959ac48847b03cc1265962cf99a8ec8a85900c087dabb30077298c66c
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
C1CCNCC1
[C:1]-[C:2](=[O;D1;H0:3])-[C:4]-[CH;D3;+0:5](-[OH;D1;+0:6])-[C:7]-[C;D1;H3:8]>>[C:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C;H0;D3;+0:5](=[O;H0;D1;+0:6])-[C:7]-[C;D1;H3:8]
56.6
[{"value": 56.6, "product": "COC1(CCN(CC1)C(=O)OC(C)(C)C)C(CC(CC)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
5
MINUTE
To a solution of oxalyl chloride (0.168 mL, 1.92 mmol) in dichloromethane (10 mL) at −78° C. was slowly added dimethyl sulfoxide (0.272 mL, 3.84 mmol). After 5 min, a solution of tert-butyl 4-(3-hydroxy-1-oxopent-1-yl)-4-methoxypiperidine-1-carboxylate (0.404 g, 1.28 mmol) from Step B in dichloromethane (5 mL) was adde...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
null
null
C1CC[NH]CC1
null
ClCCl
-78
0.083333
CCC(O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1>ClCCl>CCC(=O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-18eecdd894a74a9f87c65b58f6dc5b31
CCC(=O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1.CS(=O)(=O)N=[N+]=[N-]>>CCC(=O)C(=[N+]=[N-])C(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
S(=O)(=O)(C)N=[N+]=[N-].COC1(CCN(CC1)C(=O)OC(C)(C)C)C(CC(CC)=O)=O.C(C)N(CC)CC.S(=O)(=O)(C)N=[N+]=[N-].[OH-].[Na+]>>COC1(CCN(CC1)C(=O)OC(C)(C)C)C(C(C(CC)=O)=[N+]=[N-])=O
[CH3:1][CH2:2][C:3](=[O:4])[CH2:5][C:8](=[O:9])[C:10]1([O:11][CH3:12])[CH2:13][CH2:14][N:15]([C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])[CH2:23][CH2:24]1.CS(=O)(=O)N=[N+:6]=[N-:7]>>[CH3:1][CH2:2][C:3](=[O:4])[C:5](=[N+:6]=[N-:7])[C:8](=[O:9])[C:10]1([O:11][CH3:12])[CH2:13][CH2:14][N:15]([C:16](=[O:17])[O:1...
CCC(=O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1.CS(=O)(=O)N=[N+]=[N-]
CCC(=O)C(=[N+]=[N-])C(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
null
null
ClCCl
Heteroatom Alkylation and Arylation
OtherReaction
f358b81561b63628a435536c95a58e24369f7410be3aef157399b9be06e39ab4
2b9143c475c316d66255d8905b2d10a18b2a882ea82323797903eb2242ddbe89
C1CCNCC1
C-S(=O)(=O)-N=[N+;H0;D2:1]=[N;-;D1;H0:2].[C:3]-[C:4](=[O;D1;H0:5])-[CH2;D2;+0:6]-[C:7](-[C:8])=[O;D1;H0:9]>>[C:3]-[C:4](=[O;D1;H0:5])-[C;H0;D3;+0:6](=[N+;H0;D2:1]=[N;-;D1;H0:2])-[C:7](-[C:8])=[O;D1;H0:9]
70.8
[{"value": 70.8, "product": "COC1(CCN(CC1)C(=O)OC(C)(C)C)C(C(C(CC)=O)=[N+]=[N-])=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3.5
HOUR
To a solution of tert-butyl 4-methoxy-4-(1,3-dioxopent-1-yl)piperidine-1-carboxylate (0.227 g, 0.724 mmol) from Step C in dichloromethane (10 mL) was added triethylamine (0.101 mL, 0.724 mmol). Next, a solution of mesyl azide (0.087 g, 0.724 mmol) in dichloromethane (1 mL) was added. The reaction mixture was stirred fo...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone.Azide
Ketone.Ketone.Diazo
null
null
C1CC[NH]CC1
HO-
ClCCl
null
3.5
CCC(=O)CC(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1.CS(=O)(=O)N=[N+]=[N-]>ClCCl>CCC(=O)C(=[N+]=[N-])C(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-877888e2a7554dd4b0bc69673d1bcb3a
CCC(=O)C(=[N+]=[N-])C(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1>>CCC(=O)C1COC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
COC1(CCN(CC1)C(=O)OC(C)(C)C)C(C(C(CC)=O)=[N+]=[N-])=O>>O=C1C(COC12CCN(CC2)C(=O)OC(C)(C)C)C(CC)=O
[N-]=[N+]=[C:5]([C:3]([CH2:2][CH3:1])=[O:4])[C:21]([C:8]1([O:7][CH3:6])[CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]1)=[O:22]>>[CH3:1][CH2:2][C:3](=[O:4])[CH:5]1[CH2:6][O:7][C:8]2([CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:...
CCC(=O)C(=[N+]=[N-])C(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1
CCC(=O)C1COC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
null
CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].[Rh+2].[Rh+2]
ClCCl.Cl
C-C Coupling
OtherReaction
b2189da653e23c552f6068c1da0f8f076fd3f7e4bcbb39d3445080dac356b3a3
19d22f448f5253959cc773014604735a9b26e6bbe34e776b92a0afbc2264fb46
O=C1CCOC12CCNCC2
[C:1]-[C:2](=[O;D1;H0:3])-[C;H0;D3;+0:4](=[N+]=[N-])-[C:5](=[O;D1;H0:6])-[C:7]-[#8:8]-[CH3;D1;+0:9]>>[C:1]-[C:2](=[O;D1;H0:3])-[CH;D3;+0:4]1-[CH2;D2;+0:9]-[#8:8]-[C:7]-[C:5]-1=[O;D1;H0:6]
40.4
[{"value": 40.4, "product": "O=C1C(COC12CCN(CC2)C(=O)OC(C)(C)C)C(CC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of rhodium acetate dimer (0.002 g, 0.005 mmol) in dichloromethane (27 mL) was heated to 81° C. A solution of tert-butyl 4-methoxy-4-(2-diazo-1,3-dioxopent-1-yl)piperidine-1-carboxylate (0.092 g, 0.270 mmol) from Step D in dichloromethane (7 mL) was added slowly dropwise over 12 min. The reaction mixture was ...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone.Ether.Diazo
Ketone.Ketone.Ether
null
C1COC2(C1)CC[NH]CC2
C1COC2(C1)CC[NH]CC2
Other
CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].[Rh+2].[Rh+2].ClCCl.Cl
null
null
CCC(=O)C(=[N+]=[N-])C(=O)C1(OC)CCN(C(=O)OC(C)(C)C)CC1>CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].[Rh+2].[Rh+2].ClCCl.Cl>CCC(=O)C1COC2(CCN(C(=O)OC(C)(C)C)CC2)C1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6fc8772e8a914fc196de9870a1e7a81f
C=CC1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2>>CC(C)(C)OC(=O)N1CCC2(CCC(=O)C2C=O)CC1
O=[O+][O-].C(=C)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)=O>>C(=O)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)=O
C=[CH:17][CH:16]1[C:11]2([CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:20][CH2:19]2)[CH2:12][CH2:13][C:14]1=[O:15]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]2([CH2:12][CH2:13][C:14](=[O:15])[CH:16]2[CH:17]=[O:18])[CH2:19][CH2:20]1
C=CC1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2
CC(C)(C)OC(=O)N1CCC2(CCC(=O)C2C=O)CC1
null
null
CO
Oxidation
Alkene oxidation to aldehyde
d8a9b78d3268b1276aae5339f679b7d52c3239349ff909dd02d119f9b6b6fbf6
63e1c45bed9e5e455511d54aa776987c80b93229f60232b32aa30b9f700d26d1
O=C1CCC2(CCNCC2)C1
C=[CH;D2;+0:1]-[C:2](-[C:3])-[C:4](=[O;D1;H0:5])-[C:6]>>[C:3]-[C:2](-[CH;D2;+0:1]=[O;D1;H0:7])-[C:4](=[O;D1;H0:5])-[C:6]
null
[]
null
null
null
null
Ozone was bubbled into a solution of tert-butyl 1-vinyl-2-oxo-8-azaspiro[4.5]decane-8-carboxylate (0.168 g, 0.599 mmol) from Step B in methanol (6 mL) at −70° C. until a blue color persisted. Excess ozone was removed with a stream of nitrogen and then dimethyl sulfide (0.5 mL) was added. The mixture was allowed to warm...
10.6084/m9.figshare.5104873.v1
null
Vinyl
Aldehyde
null
null
C1CCC2(C1)CC[NH]CC2
null
CO
null
null
C=CC1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2>CO>CC(C)(C)OC(=O)N1CCC2(CCC(=O)C2C=O)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c841e5b9f76e464caf7e47b43aa62af9
C=CC1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2>>C=CC1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2
C(=C)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)=O.[BH4-].[Na+]>>C(=C)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O
[CH2:1]=[CH:2][CH:3]1[C:4](=[O:5])[CH2:6][CH2:7][C:8]12[CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]2>>[CH2:1]=[CH:2][CH:3]1[CH:4]([OH:5])[CH2:6][CH2:7][C:8]12[CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]2
C=CC1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2
C=CC1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2
null
null
CO
Reduction
Reduction of ketone to secondary alcohol
436995e4b29546c77ec774184ce22ee76b939a31d8b42f590afcb0d9fcf0ad91
1bd3cd74b454139c0a0068ac0135836499926b274bff569df163210c6c944a89
C1CCC2(C1)CCNCC2
[C;D1;H2:1]=[C:2]-[C:3]1-[C:4]-[C:5]-[C:6]-[C;H0;D3;+0:7]-1=[O;H0;D1;+0:8]>>[C;D1;H2:1]=[C:2]-[C:3]1-[C:4]-[C:5]-[C:6]-[CH;D3;+0:7]-1-[OH;D1;+0:8]
104.6
[{"value": 104.6, "product": "C(=C)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of tert-butyl 1-vinyl-2-oxo-8-azaspiro[4.5]decane-8-carboxylate (0.59 g, 2.11 mmol) from Procedure 17, Step B in methanol (6 mL) was cooled to −70° C. and sodium borohydride (0.022 g, 0.60 mmol) was added. The reaction was allowed to warm to room temperature for 3 h and was then quenched with the addition of...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
null
CO
null
null
C=CC1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2>CO>C=CC1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9ec86a96bfa746418eba080ec0d772d5
C=CC1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2.CC(C)(C)[Si](C)(C)Cl>>C=CC1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2
[Si](C)(C)(C(C)(C)C)Cl.C(=C)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O.N1C=NC=C1>>C(=C)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O[Si](C)(C)C(C)(C)C
[CH2:1]=[CH:2][CH:3]1[CH:4]([OH:5])[CH2:13][CH2:14][C:15]12[CH2:16][CH2:17][N:18]([C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])[CH2:26][CH2:27]2.Cl[Si:6]([CH3:7])([CH3:8])[C:9]([CH3:10])([CH3:11])[CH3:12]>>[CH2:1]=[CH:2][CH:3]1[CH:4]([O:5][Si:6]([CH3:7])([CH3:8])[C:9]([CH3:10])([CH3:11])[CH3:12])[CH2:13][CH2...
C=CC1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2.CC(C)(C)[Si](C)(C)Cl
C=CC1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2
null
null
C([O-])(O)=O.[Na+].CN(C)C=O.CCOCC
Protection
Alcohol protection with silyl ethers
e19079a85b3e2f818dbb25a774b915f0e7349126f5b76d72c22f1c90edfa8480
16de9d9d08d1cc67ec96e76fc213a6b49c0af7979ac901a377ee705ba5071899
C1CCC2(C1)CCNCC2
Cl-[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;D1;H2:13]>>[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;D1;H2:13]
86.2
[{"value": 86.2, "product": "C(=C)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O[Si](C)(C)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
To a solution of tert-butyl 1-vinyl-2-hydroxy-8-azaspiro[4.5]decane-8-carboxylate (0.462 g, 1.64 mmoL) from Step A in DMF (8 mL) was added imidazole (0.335 mg, 4.92 mmol) and then tert-butyldimethylsilyl chloride (0.370 g, 2.4 mmol). The reaction was stirred at room temperature for 20 h and then diluted with ether and ...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Silyl protective group
TMS ether protective group
null
null
C1CCC2(C1)CC[NH]CC2
HCl
C([O-])(O)=O.[Na+].CN(C)C=O.CCOCC
null
20
C=CC1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2.CC(C)(C)[Si](C)(C)Cl>C([O-])(O)=O.[Na+].CN(C)C=O.CCOCC>C=CC1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b6b06fbe021c44f3b8106057062933c8
CC(C)(C)OC(=O)N1CCC2(CCC(O[Si](C)(C)C(C)(C)C)C2C=O)CC1>>CCC(O)C1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2
C([O-])(O)=O.[Na+].C(C)[Mg]Br.C(=O)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O[Si](C)(C)C(C)(C)C.C(C)[Mg]Br>>OC(CC)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O[Si](C)(C)C(C)(C)C
[CH:3](=[O:4])[CH:5]1[CH:6]([O:7][Si:8]([CH3:9])([CH3:10])[C:11]([CH3:12])([CH3:13])[CH3:14])[CH2:15][CH2:16][C:17]12[CH2:18][CH2:19][N:20]([C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27])[CH2:28][CH2:29]2>>[CH3:1][CH2:2][CH:3]([OH:4])[CH:5]1[CH:6]([O:7][Si:8]([CH3:9])([CH3:10])[C:11]([CH3:12])([CH3:13])[CH3:14...
CC(C)(C)OC(=O)N1CCC2(CCC(O[Si](C)(C)C(C)(C)C)C2C=O)CC1
CCC(O)C1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2
null
null
C1CCOC1.CCOCC
Miscellaneous
OtherReaction
1ffaf80f172e20da969364a5d2977299bc51b204f2262675c45c8ec58ff36ac0
e005d650d08e61fc67b766830eb53235a9bc084cc3667d2f8a73c2fb8bb34277
C1CCC2(C1)CCNCC2
[C:1]-[C:2](-[CH;D2;+0:3]=[O;H0;D1;+0:4])-[C:5]>>[C:1]-[C:2](-[CH;D3;+0:3](-[OH;D1;+0:4])-[C:6]-[C;D1;H3:7])-[C:5]
81.2
[{"value": 81.2, "product": "OC(CC)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O[Si](C)(C)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A solution of tert-butyl 1-formyl-2-(tert-butyldimethylsilyloxy)-8-azaspiro[4.5]decane-8-carboxylate (0.284 g, 0.714 mmol) from Step C in THF (7 mL) was cooled to −70° C. and ethyl magnesium bromide (3.0M, 0.262 mL, 0.786 mmol) was added. The reaction was stirred for 30 min and then an additional aliquot of ethyl magne...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Secondary alcohol
null
null
C1CCC2(C1)CC[NH]CC2
Other
C1CCOC1.CCOCC
null
0.5
CC(C)(C)OC(=O)N1CCC2(CCC(O[Si](C)(C)C(C)(C)C)C2C=O)CC1>C1CCOC1.CCOCC>CCC(O)C1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-93cc11062a204c5dbc59f3d76e2c7a2a
CCC(O)C1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2>>CCC(O)C1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2
OC(CC)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O[Si](C)(C)C(C)(C)C.[F-].C(CCC)[N+](CCCC)(CCCC)CCCC>>OC(CC)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O
CC(C)(C)[Si](C)(C)[O:7][CH:6]1[CH:5]([CH:3]([CH2:2][CH3:1])[OH:4])[C:10]2([CH2:9][CH2:8]1)[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:21][CH2:22]2>>[CH3:1][CH2:2][CH:3]([OH:4])[CH:5]1[CH:6]([OH:7])[CH2:8][CH2:9][C:10]12[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])(...
CCC(O)C1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2
CCC(O)C1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2
null
null
C1CCOC1.C(C)(=O)OCC.Cl
Deprotection
Alcohol deprotection from silyl ethers
050b4fb4e1e9936189860d27dded10ae70a294a642c52f800eb9d5aaef7955cc
88623e19d23cdfe8e1a4c167fd6cfc51d774a1c784b87a7bb2df8153ee93e67a
C1CCC2(C1)CCNCC2
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[OH;D1;+0:1])-[C:4]
99
[{"value": 99.0, "product": "OC(CC)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
To a solution of tert-butyl 1-(1-hydroxyprop-1-yl)-2-(tert-butyldimethylsilyloxy)-8-azaspiro[4.5]decane-8-carboxylate (0.248 g, 0.58 mmol) in THF (15 mL) was added 1M tetrabutylammonium fluoride in THF (2.3 mL, 2.3 mmol). The solution was stirred at room temperature for 4 h and was then diluted with ethyl acetate, pour...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Secondary alcohol
null
null
C1CCC2(C1)CC[NH]CC2
Other
C1CCOC1.C(C)(=O)OCC.Cl
null
4
CCC(O)C1C(O[Si](C)(C)C(C)(C)C)CCC12CCN(C(=O)OC(C)(C)C)CC2>C1CCOC1.C(C)(=O)OCC.Cl>CCC(O)C1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e1ccb3f7a4454efaa02b3ba0424b4745
CCC(O)C1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2>>CCC(=O)C1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2
OC(CC)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)O.CC(=O)C.OS(=O)(=O)O.O=[Cr](=O)=O>>O=C(CC)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)=O
[CH3:1][CH2:2][CH:3]([OH:4])[CH:5]1[CH:6]([OH:7])[CH2:8][CH2:9][C:10]12[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:21][CH2:22]2>>[CH3:1][CH2:2][C:3](=[O:4])[CH:5]1[C:6](=[O:7])[CH2:8][CH2:9][C:10]12[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH...
CCC(O)C1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2
CCC(=O)C1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2
null
null
CC(=O)C
Oxidation
OtherReaction
ea7d092d21dc7125486e9b2efcd7f66954cd05df4007b8b9d4fa83bb8b8a9165
784b65917ae952abb76a69fc81990586d899be4ce8f5fa5c24fb1cb70b659234
O=C1CCC2(CCNCC2)C1
[C;D1;H3:1]-[C:2]-[CH;D3;+0:3](-[OH;D1;+0:4])-[C:5]1-[C:6]-[C:7]-[C:8]-[CH;D3;+0:9]-1-[OH;D1;+0:10]>>[C;D1;H3:1]-[C:2]-[C;H0;D3;+0:3](=[O;H0;D1;+0:4])-[C:5]1-[C:6]-[C:7]-[C:8]-[C;H0;D3;+0:9]-1=[O;H0;D1;+0:10]
66.7
[{"value": 66.7, "product": "O=C(CC)C1C(CCC12CCN(CC2)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a solution of tert-butyl 1-(1-hydroxyprop-1-yl)-2-hydroxy-8-azaspiro[4.5]decane-8-carboxylate (0.050 g, 0.16 mmol) from Step E in acetone (2 mL) at 0° C. was added 2.6M Jones reagent (0.122 mL, 0.32 mmol). The reaction was stirred at room temperature for 10 min and was then quenched with isopropanol. The mixture was...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Secondary alcohol
Ketone.Ketone
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
C1CCC2(C1)CC[NH]CC2
null
CC(=O)C
null
0.166667
CCC(O)C1C(O)CCC12CCN(C(=O)OC(C)(C)C)CC2>CC(=O)C>CCC(=O)C1C(=O)CCC12CCN(C(=O)OC(C)(C)C)CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d0cc87cbef5e40de9f67dab66499498b
CC(C)(C)[Si](C)(C)OCCBr.COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1>>COC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
C([O-])(O)=O.[Na+].C[Si](C)(C)[N-][Si](C)(C)C.[K+].COC(=O)C1CCN(CC1)C(=O)OC(C)(C)C.BrCCO[Si](C)(C)C(C)(C)C>>COC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C
Br[CH2:6][CH2:7][O:8][Si:9]([CH3:10])([CH3:11])[C:12]([CH3:13])([CH3:14])[CH3:15].[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:16][CH2:17][N:18]([C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])[CH2:26][CH2:27]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][CH2:7][O:8][Si:9]([CH3:10])([CH3:11])[C:12]([CH3:13])([CH3:14])[CH3:...
CC(C)(C)[Si](C)(C)OCCBr.COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1
COC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
null
null
C1CCOC1
C-C Coupling
OtherReaction
cc17dfd0def644ca87e815e637357310f207eb90d8b3273b51858e3602d79eca
0061a06af9fc64155952582b91b574e4abd8908ca14244f15179c2400b24dd08
C1CCNCC1
Br-[CH2;D2;+0:1]-[C:2]-[#8:3].[C;D1;H3:4]-[#8:5]-[C:6](=[O;D1;H0:7])-[CH;D3;+0:8]1-[C:9]-[C:10]-[#7:11]-[C:12]-[C:13]-1>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[C;H0;D4;+0:8]1(-[C:6](=[O;D1;H0:7])-[#8:5]-[C;D1;H3:4])-[C:9]-[C:10]-[#7:11]-[C:12]-[C:13]-1
null
[]
null
null
1
HOUR
To a solution of KHMDS (8.72 g, 44 mmol) in THF (300 mL) at −70° C. was slowly added over 10 min a solution of tert-butyl 4-methoxycarbonylpiperidine-1-carboxylate (7.1 g, 29 mmol) in THF (70 mL). After 1 h, 2-bromo-1-(tert-butyldimethylsilyloxy)ethane (10 g, 47 mmol) was added and the reaction was allowed to warm to r...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester
Ester
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1
HBr
C1CCOC1
null
1
CC(C)(C)[Si](C)(C)OCCBr.COC(=O)C1CCN(C(=O)OC(C)(C)C)CC1>C1CCOC1>COC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0677070e85e2467c947e5de20344088b
COC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1>>CC(C)(C)OC(=O)N1CCC(CO)(CCO[Si](C)(C)C(C)(C)C)CC1
[BH4-].[Li+].COC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C.[BH4-].[Li+]>>OCC1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C
CO[C:12]([C:11]1([CH2:14][CH2:15][O:16][Si:17]([CH3:18])([CH3:19])[C:20]([CH3:21])([CH3:22])[CH3:23])[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:25][CH2:24]1)=[O:13]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]([CH2:12][OH:13])([CH2:14][CH2:15][O:16][Si:17]...
COC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
CC(C)(C)OC(=O)N1CCC(CO)(CCO[Si](C)(C)C(C)(C)C)CC1
null
null
C1CCOC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
C1CCNCC1
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3](-[C:4])(-[C:5])-[C:6]>>[C:5]-[C:3](-[C:4])(-[CH2;D2;+0:1]-[OH;D1;+0:2])-[C:6]
null
[]
null
null
2
DAY
The crude tert-butyl 4-methoxycarbonyl-4-(2-(tert-butyldimethylsilyloxy)eth-1-yl)piperidine-1-carboxylate (assumed 44 mmol) from Step A was taken up in THF (200 mL) and 2M lithium borohydride in THF (29 mL, 58 mmol) was added via syringe at room temperature. The reaction was stirred for 2 days at room temperature and t...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
C1CC[NH]CC1
Other
C1CCOC1
null
48
COC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1>C1CCOC1>CC(C)(C)OC(=O)N1CCC(CO)(CCO[Si](C)(C)C(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4bd35abee2ce4dad988436debf719e15
CC(C)(C)OC(=O)N1CCC(CO)(CCO[Si](C)(C)C(C)(C)C)CC1>>CC(C)(C)OC(=O)N1CCC(C=O)(CCO[Si](C)(C)C(C)(C)C)CC1
C(C)N(CC)CC.OCC1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C.C(C(=O)Cl)(=O)Cl.CS(=O)C>>C(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]([CH2:12][OH:13])([CH2:14][CH2:15][O:16][Si:17]([CH3:18])([CH3:19])[C:20]([CH3:21])([CH3:22])[CH3:23])[CH2:24][CH2:25]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]([CH:12]=[O:13])([CH2:14][CH2:15][O:16][Si:17]([C...
CC(C)(C)OC(=O)N1CCC(CO)(CCO[Si](C)(C)C(C)(C)C)CC1
CC(C)(C)OC(=O)N1CCC(C=O)(CCO[Si](C)(C)C(C)(C)C)CC1
null
null
O.C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
C1CCNCC1
[C:1]-[C:2](-[C:3])(-[CH2;D2;+0:4]-[OH;D1;+0:5])-[C:6]>>[C:1]-[C:2](-[C:3])(-[CH;D2;+0:4]=[O;H0;D1;+0:5])-[C:6]
89.2
[{"value": 89.2, "product": "C(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To a solution of oxalyl chloride (3.3 mL, 38 mmol) in methylene chloride (500 mL) at −70° C. was added DMSO (5.4 mL, 76 mmol) over 5 min. After 15 min, a solution of tert-butyl 4-hydroxymethyl-4-(2-(tert-butyldimethylsilyloxy)eth-1-yl)piperidine-1-carboxylate (7.1 g, 19 mmol) in methylene chloride (125 mL) was slowly a...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
C1CC[NH]CC1
null
O.C(Cl)Cl
null
0.25
CC(C)(C)OC(=O)N1CCC(CO)(CCO[Si](C)(C)C(C)(C)C)CC1>O.C(Cl)Cl>CC(C)(C)OC(=O)N1CCC(C=O)(CCO[Si](C)(C)C(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f72326cb43594b419689d372b0652184
CC(C)(C)OC(=O)N1CCC(C=O)(CCO[Si](C)(C)C(C)(C)C)CC1>>CC(O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
C([O-])(O)=O.[Na+].C[Li].C(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C.C[Li]>>OC(C)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C
[CH:2](=[O:3])[C:4]1([CH2:5][CH2:6][O:7][Si:8]([CH3:9])([CH3:10])[C:11]([CH3:12])([CH3:13])[CH3:14])[CH2:15][CH2:16][N:17]([C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[CH2:25][CH2:26]1>>[CH3:1][CH:2]([OH:3])[C:4]1([CH2:5][CH2:6][O:7][Si:8]([CH3:9])([CH3:10])[C:11]([CH3:12])([CH3:13])[CH3:14])[CH2:15][CH2:16...
CC(C)(C)OC(=O)N1CCC(C=O)(CCO[Si](C)(C)C(C)(C)C)CC1
CC(O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
null
null
C1CCOC1.CCOCC
Miscellaneous
OtherReaction
1ffaf80f172e20da969364a5d2977299bc51b204f2262675c45c8ec58ff36ac0
e005d650d08e61fc67b766830eb53235a9bc084cc3667d2f8a73c2fb8bb34277
C1CCNCC1
[C:1]-[C:2](-[C:3])(-[CH;D2;+0:4]=[O;H0;D1;+0:5])-[C:6]>>[C:1]-[C:2](-[C:3])(-[CH;D3;+0:4](-[C;D1;H3:7])-[OH;D1;+0:5])-[C:6]
null
[]
null
null
2
HOUR
To a solution of tert-butyl 4-formyl-4-(2-(tert-butyldimethylsilyloxy)eth-1-yl)piperidine-1-carboxylate (6.3 g, 17 mmol) in THF (170 mL) at −70° C. was added 1.4M methyl lithium in ether (13.3 mL, 19 mmol). After 2 h, an additional amount of 1.4M methyl lithium in ether (2.5 mL) was added. After an additional 30 min, t...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Secondary alcohol
null
null
C1CC[NH]CC1
Other
C1CCOC1.CCOCC
null
2
CC(C)(C)OC(=O)N1CCC(C=O)(CCO[Si](C)(C)C(C)(C)C)CC1>C1CCOC1.CCOCC>CC(O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8f33fd77764b4fe7a6059f8325c13e1b
CC(O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1>>CC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
C(C)N(CC)CC.OC(C)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C.C(C(=O)Cl)(=O)Cl.CS(=O)C>>C(C)(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C
[CH3:1][CH:2]([OH:3])[C:4]1([CH2:5][CH2:6][O:7][Si:8]([CH3:9])([CH3:10])[C:11]([CH3:12])([CH3:13])[CH3:14])[CH2:15][CH2:16][N:17]([C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[CH2:25][CH2:26]1>>[CH3:1][C:2](=[O:3])[C:4]1([CH2:5][CH2:6][O:7][Si:8]([CH3:9])([CH3:10])[C:11]([CH3:12])([CH3:13])[CH3:14])[CH2:15][...
CC(O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
CC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
null
null
O.C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
c7c20d2959ac48847b03cc1265962cf99a8ec8a85900c087dabb30077298c66c
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
C1CCNCC1
[C:1]-[C:2](-[C:3])(-[CH;D3;+0:4](-[C;D1;H3:5])-[OH;D1;+0:6])-[C:7]>>[C:1]-[C:2](-[C:3])(-[C;H0;D3;+0:4](-[C;D1;H3:5])=[O;H0;D1;+0:6])-[C:7]
68.6
[{"value": 68.6, "product": "C(C)(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To a solution of oxalyl chloride (3.0 mL, 34 mmol) in methylene chloride (400 mL) at −70° C. was added DMSO (4.8 mL, 68 mmol) over 5 min. After 15 min, a solution of tert-butyl 4-(1-hydroxyeth-1-yl)-4-(2-(tert-butyldimethylsilyloxy)eth-1-yl)piperidine-1-carboxylate (6.6 g, 17 mmol) in methylene chloride (125 mL) was sl...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
null
null
C1CC[NH]CC1
null
O.C(Cl)Cl
null
0.25
CC(O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1>O.C(Cl)Cl>CC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-25b347290fcb4197b31ab076516a514a
CC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1.O=CCc1ccccc1>>CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(O)Cc2ccccc2)CC1
[Cl-].[NH4+].C1(=CC=CC=C1)CC=O.C(C)(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C.CN(C)P(=O)(N(C)C)N(C)C.[Li+].C[Si](C)(C)[N-][Si](C)(C)C>>C1(=CC=CC=C1)CC(CC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C)O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]([CH2:12][CH2:13][O:14][Si:15]([CH3:16])([CH3:17])[C:18]([CH3:19])([CH3:20])[CH3:21])([C:22](=[O:23])[CH3:24])[CH2:34][CH2:35]1.[CH:25](=[O:26])[CH2:27][c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])...
CC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1.O=CCc1ccccc1
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(O)Cc2ccccc2)CC1
null
null
C1CCOC1.CCOCC
C-C Coupling
OtherReaction
d08eb7b2615717189cce315501bb2cfa7ee3668e6d8eaa24218b092d1454a850
7d7139092067ff475e8e8a4ad6adb4833600ca969e282ed08dc56c016dccb864
O=C(CCCc1ccccc1)C1CCNCC1
[C:1]-[C:2](-[CH3;D1;+0:3])=[O;D1;H0:4].[O;H0;D1;+0:5]=[CH;D2;+0:6]-[C:7]-[c:8]>>[C:1]-[C:2](=[O;D1;H0:4])-[CH2;D2;+0:3]-[CH;D3;+0:6](-[OH;D1;+0:5])-[C:7]-[c:8]
null
[]
null
null
1
HOUR
To a solution of tert-butyl 4-acetyl-4-(2-(tert-butyldimethylsilyloxy)eth-1-yl)piperidine-1-carboxylate (4.6 g, 12 mmol) in THF (120 mL) at −70° C. was added HMPA (20.7 mL, 120 mmol) and 1M LHMDS in THF (12 mL, 12 mmol). After 1 h, phenylacetaldehyde (5.7 g, 48 mmol) was added in THF (80 mL) over 10 min and the reactio...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone.Secondary alcohol
null
null
C1CC[NH]CC1.c1ccccc1
null
C1CCOC1.CCOCC
null
1
CC(=O)C1(CCO[Si](C)(C)C(C)(C)C)CCN(C(=O)OC(C)(C)C)CC1.O=CCc1ccccc1>C1CCOC1.CCOCC>CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(O)Cc2ccccc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0ad6df59fec94b07b829b6f097e8956d
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(O)Cc2ccccc2)CC1>>CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(=O)Cc2ccccc2)CC1
C1(=CC=CC=C1)CC(CC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C)O.CC(=O)OI1(C=2C=CC=CC2C(=O)O1)(OC(=O)C)OC(=O)C>>C1(=CC=CC=C1)CC(CC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]([CH2:12][CH2:13][O:14][Si:15]([CH3:16])([CH3:17])[C:18]([CH3:19])([CH3:20])[CH3:21])([C:22](=[O:23])[CH2:24][CH:25]([OH:26])[CH2:27][c:28]2[cH:29][cH:30][cH:31][cH:32][cH:33]2)[CH2:34][CH2:35]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[...
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(O)Cc2ccccc2)CC1
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(=O)Cc2ccccc2)CC1
null
null
C(Cl)Cl.CCOCC
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
c7c20d2959ac48847b03cc1265962cf99a8ec8a85900c087dabb30077298c66c
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
O=C(CC(=O)C1CCNCC1)Cc1ccccc1
[C:1]-[C:2](=[O;D1;H0:3])-[C:4]-[CH;D3;+0:5](-[OH;D1;+0:6])-[C:7]-[c:8]>>[C:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C;H0;D3;+0:5](=[O;H0;D1;+0:6])-[C:7]-[c:8]
69.5
[{"value": 69.5, "product": "C1(=CC=CC=C1)CC(CC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a solution of tert-butyl 4-(4-phenyl-3-hydroxy-1-oxobut-1-yl)-4-(2-(tert-butyldimethylsilyloxy)eth-1-yl)piperidine-1-carboxylate (494 mg, 0.98 mmol) from Step F in methylene chloride (10 mL) at room temperature was added Dess-Martin reagent (621 mg, 1.5 mmol). After 3 h, the reaction was diluted with ether and quenc...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
null
null
C1CC[NH]CC1.c1ccccc1
null
C(Cl)Cl.CCOCC
null
3
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(O)Cc2ccccc2)CC1>C(Cl)Cl.CCOCC>CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(=O)Cc2ccccc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b1cbf72bde5741aa9e5793f4199bac7c
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(=O)Cc2ccccc2)CC1.NN>>CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(c2cc(Cc3ccccc3)n[nH]2)CC1
C1(=CC=CC=C1)CC(CC(=O)C1(CCN(CC1)C(=O)OC(C)(C)C)CCO[Si](C)(C)C(C)(C)C)=O.O.NN>>C(C)(C)(C)OC(=O)N1CCC(CC1)(C1=CC(=NN1)CC1=CC=CC=C1)CCO[Si](C)(C)C(C)(C)C
O=[C:22]([C:11]1([CH2:12][CH2:13][O:14][Si:15]([CH3:16])([CH3:17])[C:18]([CH3:19])([CH3:20])[CH3:21])[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:35][CH2:34]1)[CH2:23][C:24](=O)[CH2:25][c:26]1[cH:27][cH:28][cH:29][cH:30][cH:31]1.[NH2:32][NH2:33]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[...
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(=O)Cc2ccccc2)CC1.NN
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(c2cc(Cc3ccccc3)n[nH]2)CC1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
96717cf3e91d029570228ab77c24b1373a8a647af1e168bf2ca95f0bd5bf6ad5
d14f370ee7ee5e4a5c5c7412f191c74a005faab09898998e0db4b3670a6f4f81
c1ccc(Cc2cc(C3CCNCC3)[nH]n2)cc1
O=[C;H0;D3;+0:1](-[CH2;D2;+0:2]-[C;H0;D3;+0:3](=O)-[C:4]-[c:5])-[C:6](-[C:7])(-[C:8])-[C:9].[NH2;D1;+0:10]-[NH2;D1;+0:11]>>[C:8]-[C:6](-[C:7])(-[c;H0;D3;+0:1]1:[cH;D2;+0:2]:[c;H0;D3;+0:3](-[C:4]-[c:5]):[n;H0;D2;+0:10]:[nH;D2;+0:11]:1)-[C:9]
71.5
[{"value": 71.5, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)(C1=CC(=NN1)CC1=CC=CC=C1)CCO[Si](C)(C)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
To a solution of tert-butyl 4-(4-phenyl-1,3-dioxobut-1-yl)-4-(2-(tert-butyldimethylsilyloxy)eth-1-yl)piperidine-1-carboxylate (343 mg, 0.68 mmol) from Step G in ethanol (7 mL) was added hydrazine hydrate (0.040 mL, 0.82 mmol). The reaction was heated at 85° C. for 3 h and was then concentrated in vacuo. The residue was...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ketone
null
null
c1cn[nH]c1
C1CC[NH]CC1.c1cn[nH]c1.c1ccccc1
HO-
C(C)O
85
null
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(C(=O)CC(=O)Cc2ccccc2)CC1.NN>C(C)O>CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(c2cc(Cc3ccccc3)n[nH]2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-22577971d76249afb71b0146d403c604
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(c2cc(Cc3ccccc3)n[nH]2)CC1>>CC(C)(C)OC(=O)N1CCC(CCO)(c2cc(Cc3ccccc3)n[nH]2)CC1
C(C)(C)(C)OC(=O)N1CCC(CC1)(C1=CC(=NN1)CC1=CC=CC=C1)CCO[Si](C)(C)C(C)(C)C.[F-].C(CCC)[N+](CCCC)(CCCC)CCCC.Cl>>C(C)(C)(C)OC(=O)N1CCC(CC1)(C1=CC(=NN1)CC1=CC=CC=C1)CCO
CC(C)(C)[Si](C)(C)[O:14][CH2:13][CH2:12][C:11]1([c:15]2[cH:16][c:17]([CH2:18][c:19]3[cH:20][cH:21][cH:22][cH:23][cH:24]3)[n:25][nH:26]2)[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:28][CH2:27]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]([CH2:12][CH2:13][OH...
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(c2cc(Cc3ccccc3)n[nH]2)CC1
CC(C)(C)OC(=O)N1CCC(CCO)(c2cc(Cc3ccccc3)n[nH]2)CC1
null
null
C1CCOC1.C(C)(=O)OCC
Deprotection
Alcohol deprotection from silyl ethers
6ff8c9c41093ab5237b871dd4689ba6431022d615e227d3774901a983c846e4b
84d9f5b4e7757c58e584c26c7d52c9a3f594fbcb0c0d22f34765a93a932fcd5b
c1ccc(Cc2cc(C3CCNCC3)[nH]n2)cc1
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[OH;D1;+0:1]
66.2
[{"value": 66.2, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)(C1=CC(=NN1)CC1=CC=CC=C1)CCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 1-(tert-butoxycarbonyl)-4-(2-tert-butyldimethylsilyloxyeth-1-yl)-4-(3-benzyl-(1H)-pyrazol-5-yl)piperidine (243 mg, 0.49 mmol) from Step H in THF (5 mL) was added 1M tetrabutylammonium fluoride in THF (0.63 mL, 0.63 mmol). The reaction was stirred at room temperature for 1 h and was then diluted with et...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Primary alcohol
null
null
C1CC[NH]CC1.c1cn[nH]c1.c1ccccc1
Other
C1CCOC1.C(C)(=O)OCC
null
1
CC(C)(C)OC(=O)N1CCC(CCO[Si](C)(C)C(C)(C)C)(c2cc(Cc3ccccc3)n[nH]2)CC1>C1CCOC1.C(C)(=O)OCC>CC(C)(C)OC(=O)N1CCC(CCO)(c2cc(Cc3ccccc3)n[nH]2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-23fa4558efeb46a98b4c522d23affa0c
CC(C)(C)OC(=O)N1CCC(CCO)(c2cc(Cc3ccccc3)n[nH]2)CC1>>CC(C)(C)OC(=O)N1CCC2(CC1)CCn1nc(Cc3ccccc3)cc12
C(C)(C)(C)OC(=O)N1CCC(CC1)(C1=CC(=NN1)CC1=CC=CC=C1)CCO.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.CCOC(=O)/N=N/C(=O)OCC>>C(C)(C)(C)OC(=O)N1CCC2(CCN3N=C(C=C32)CC3=CC=CC=C3)CC1
O[CH2:15][CH2:14][C:11]1([c:27]2[nH:16][n:17][c:18]([CH2:19][c:20]3[cH:21][cH:22][cH:23][cH:24][cH:25]3)[cH:26]2)[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:13][CH2:12]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C:11]2([CH2:12][CH2:13]1)[CH2:14][CH2:15][n:16]1...
CC(C)(C)OC(=O)N1CCC(CCO)(c2cc(Cc3ccccc3)n[nH]2)CC1
CC(C)(C)OC(=O)N1CCC2(CC1)CCn1nc(Cc3ccccc3)cc12
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
833218c7f4017c2be13a67b7225b7323c9da4df321a97231afa48998818e7315
2ab4024aa17b6e89368e6fe8ee731d32c7611cb9b23de403e301e8362fea90b1
c1ccc(Cc2cc3n(n2)CCC32CCNCC2)cc1
O-[CH2;D2;+0:1]-[C:2]-[C:3]-[c:4]1:[c:5]:[c:6]:[#7;a:7]:[nH;D2;+0:8]:1>>[#7;a:7]1:[c:6]:[c:5]:[c:4]2:[n;H0;D3;+0:8]:1-[CH2;D2;+0:1]-[C:2]-[C:3]-2
85
[{"value": 85.0, "product": "C(C)(C)(C)OC(=O)N1CCC2(CCN3N=C(C=C32)CC3=CC=CC=C3)CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
To a solution of 1-(tert-butoxycarbonyl)-4-(2-hydroxyeth-1-yl)-4-(3-benzyl-(1H)-pyrazol-5-yl)piperidine (125 mg, 0.32 mmol) from Step I in THF (4 mL) at 0° C. was added triphenylphosphine (85 mg, 0.32 mmol) and DEAD (0.051 mL, 0.32 mmol). The reaction was stirred for 20 min and was then allowed to warm to room temperat...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
null
c1cn[nH]c1
c1cc2n(n1)CCC21CC[NH]CC1
c1cc2n(n1)CCC21CC[NH]CC1.c1ccccc1
HO-
C1CCOC1
null
0.333333
CC(C)(C)OC(=O)N1CCC(CCO)(c2cc(Cc3ccccc3)n[nH]2)CC1>C1CCOC1>CC(C)(C)OC(=O)N1CCC2(CC1)CCn1nc(Cc3ccccc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7a5cb637174d4ad49a54d0c4b3153ed7
C=C(COC(C)=O)C[Si](C)(C)C.COC(=O)/C=C/c1cccc(F)c1>>C=C1C[C@@H](C(=O)OC)[C@H](c2cccc(F)c2)C1
FC=1C=C(/C=C/C(=O)OC)C=CC1.C(C)(=O)OCC(=C)C[Si](C)(C)C>>C=C1C[C@H]([C@@H](C1)C(=O)OC)C1=CC(=CC=C1)F
CC(=O)O[CH2:3][C:2](=[CH2:1])[CH2:17][Si](C)(C)C.[CH:4](\[C:5](=[O:6])[O:7][CH3:8])=[CH:9]/[c:10]1[cH:11][cH:12][cH:13][c:14]([F:15])[cH:16]1>>[CH2:1]=[C:2]1[CH2:3][C@@H:4]([C:5](=[O:6])[O:7][CH3:8])[C@H:9]([c:10]2[cH:11][cH:12][cH:13][c:14]([F:15])[cH:16]2)[CH2:17]1
C=C(COC(C)=O)C[Si](C)(C)C.COC(=O)/C=C/c1cccc(F)c1
C=C1C[C@@H](C(=O)OC)[C@H](c2cccc(F)c2)C1
null
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(CCP(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=CC=C1
C1CCOC1.CCCCCC
C-C Coupling
OtherReaction
a760b47d5c9f87e43eb85d2a7bf6ac4fc7baa2780167d2a6ed0d04254a77a67a
2fba473587163766819c8b06dbebd40b4bfa0901fa09bca7745f4d7d9635e563
C=C1CC[C@H](c2ccccc2)C1
C-C(=O)-O-[CH2;D2;+0:1]-[C:2](=[C;D1;H2:3])-[CH2;D2;+0:4]-[Si](-C)(-C)-C.[C;D1;H3:5]-[#8:6]-[C:7](=[O;D1;H0:8])/[CH;D2;+0:9]=[CH;D2;+0:10]/[c:11](:[c:12]):[c:13]>>[C;D1;H2:3]=[C:2]1-[CH2;D2;+0:4]-[C@@H;D3;+0:10](-[c:11](:[c:12]):[c:13])-[C@H;D3;+0:9](-[C:7](=[O;D1;H0:8])-[#8:6]-[C;D1;H3:5])-[CH2;D2;+0:1]-1
83.9
[{"value": 83.9, "product": "C=C1C[C@H]([C@@H](C1)C(=O)OC)C1=CC(=CC=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
A mixture of methyl trans-3-fluorocinnamate (41.25 g, 229 mmol), tetrakis(triphenylphosphine) palladium(0) (18.5 g, 16 mmol), 1,2-bis(diphenylphosphino)ethane (5.5 g, 13.7 mmol), and 2-((trimethylsilyl)methyl)-2-propen-1-yl acetate (42.66 g, 229 mmol) in THF (300 mL) under nitrogen was heated to reflux for 6 h and then...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Silyl protective group
Ester
null
C1CCCC1
C1CCCC1.c1ccccc1
HO-
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(CCP(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=CC=C1.C1CCOC1.CCCCCC
null
16
C=C(COC(C)=O)C[Si](C)(C)C.COC(=O)/C=C/c1cccc(F)c1>[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(CCP(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=CC=C1.C1CCOC1.CCCCCC>C=C1C[C@@H](C(=O)OC)[C@H](c2cccc(F)c2)C...
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e31142420d854a6b93bb0fdda233b4cb
BrCC1CC1.CCOP(=O)(CC(=O)OCc1ccc(OC)cc1)OCC>>CCOP(=O)(OCC)C(CC1CC1)C(=O)OCc1ccc(OC)cc1
BrCC1CC1.[H-].[Na+].COC1=CC=C(COC(CP(=O)(OCC)OCC)=O)C=C1.C([O-])(O)=O.[Na+]>>COC1=CC=C(COC(C(CC2CC2)P(=O)(OCC)OCC)=O)C=C1
Br[CH2:10][CH:11]1[CH2:12][CH2:13]1.[CH3:1][CH2:2][O:3][P:4](=[O:5])([O:6][CH2:7][CH3:8])[CH2:9][C:14](=[O:15])[O:16][CH2:17][c:18]1[cH:19][cH:20][c:21]([O:22][CH3:23])[cH:24][cH:25]1>>[CH3:1][CH2:2][O:3][P:4](=[O:5])([O:6][CH2:7][CH3:8])[CH:9]([CH2:10][CH:11]1[CH2:12][CH2:13]1)[C:14](=[O:15])[O:16][CH2:17][c:18]1[cH:1...
BrCC1CC1.CCOP(=O)(CC(=O)OCc1ccc(OC)cc1)OCC
CCOP(=O)(OCC)C(CC1CC1)C(=O)OCc1ccc(OC)cc1
null
null
C(C)OCC.CN(C)C=O
C-C Coupling
OtherReaction
cce1a125a1ff1ac49e6bca841c71f39abbf2c962f7edb2747b8c98f3307cb502
0061a06af9fc64155952582b91b574e4abd8908ca14244f15179c2400b24dd08
O=C(CCC1CC1)OCc1ccccc1
Br-[CH2;D2;+0:1]-[C:2]1-[C:3]-[C:4]-1.[#8:5]-[#15:6](-[#8:7])(=[O;D1;H0:8])-[CH2;D2;+0:9]-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]>>[#8:5]-[#15:6](-[#8:7])(=[O;D1;H0:8])-[CH;D3;+0:9](-[CH2;D2;+0:1]-[C:2]1-[C:3]-[C:4]-1)-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]
60.9
[{"value": 60.9, "product": "COC1=CC=C(COC(C(CC2CC2)P(=O)(OCC)OCC)=O)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a suspension of 60% sodium hydride in mineral oil (0.840 g, 21.0 mmol) in DMF (100 mL) was added a solution of 2-(diethoxyphosphoryl)acetic acid 4-methoxybenzyl ester (6.04 g, 19.1 mmol) from Step A in DMF (10 mL). The reaction mixture was stirred for 30 min at room temperature. Bromomethylcyclopropane (2.4 mL, 24.8...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester
Ester
null
null
C1CC1.c1ccccc1
HBr
C(C)OCC.CN(C)C=O
null
0.5
BrCC1CC1.CCOP(=O)(CC(=O)OCc1ccc(OC)cc1)OCC>C(C)OCC.CN(C)C=O>CCOP(=O)(OCC)C(CC1CC1)C(=O)OCc1ccc(OC)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f4f5c73c0baa450b83cabe4ac2020d77
BrCc1ccccc1.C=C1C[C@@H](CO)[C@H](c2cccc(F)c2)C1>>C=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1
OC[C@H]1[C@@H](CC(C1)=C)C1=CC(=CC=C1)F.C(C1=CC=CC=C1)Br.[H-].[Na+]>>C(C1=CC=CC=C1)OC[C@@H]1[C@H](CC(C1)=C)C1=CC(=CC=C1)F
Br[CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1.[CH2:1]=[C:2]1[CH2:3][C@@H:4]([CH2:5][OH:6])[C@H:14]([c:15]2[cH:16][cH:17][cH:18][c:19]([F:20])[cH:21]2)[CH2:22]1>>[CH2:1]=[C:2]1[CH2:3][C@H:4]([CH2:5][O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[C@@H:14]([c:15]2[cH:16][cH:17][cH:18][c:19]([F:20])[cH:21]2)[CH...
BrCc1ccccc1.C=C1C[C@@H](CO)[C@H](c2cccc(F)c2)C1
C=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1
null
null
CN(C)C=O.CCOCC
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
dd3f9c60e1f90d961a7c01d970ae213561355ee1451f276a3b04696e4b6fae5c
46a6e883cf919b4006e69abfdfd883f458f55c08b3200960c6a5b57c4139fbca
C=C1C[C@H](COCc2ccccc2)[C@@H](c2ccccc2)C1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]-[OH;D1;+0:7]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
90.4
[{"value": 90.4, "product": "C(C1=CC=CC=C1)OC[C@@H]1[C@H](CC(C1)=C)C1=CC(=CC=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
To a solution of (+)-trans-1-hydroxymethyl-4-methylene-2-(3-fluorophenyl)cyclopentane (5.0 g, 26.5 mmol) from Example 1, Step C and benzyl bromide (4.7 mL, 40 mmol) in DMF (130 mL) was added 60% sodium hydride in mineral oil (0.77 g, 32 mmol). The reaction was stirred at room temperature for 24 h was then diluted with ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary alcohol
Ether
null
null
C1CCCC1.c1ccccc1.c1ccccc1
HBr
CN(C)C=O.CCOCC
null
24
BrCc1ccccc1.C=C1C[C@@H](CO)[C@H](c2cccc(F)c2)C1>CN(C)C=O.CCOCC>C=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-36b5e5b058cd4a5891c61b3f493afe55
C=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1.CO>>O=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1
C(C1=CC=CC=C1)OC[C@@H]1[C@H](CC(C1)=C)C1=CC(=CC=C1)F.CO>>C(C1=CC=CC=C1)OC[C@H]1CC(C[C@@H]1C1=CC(=CC=C1)F)=O
C=[C:2]1[CH2:3][C@H:4]([CH2:5][O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[C@@H:14]([c:15]2[cH:16][cH:17][cH:18][c:19]([F:20])[cH:21]2)[CH2:22]1.C[OH:1]>>[O:1]=[C:2]1[CH2:3][C@H:4]([CH2:5][O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[C@@H:14]([c:15]2[cH:16][cH:17][cH:18][c:19]([F:20])[cH:21]2)[CH2:22...
C=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1.CO
O=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
88ae21c3f20673f4bc27c05c339b079cc70654b9dd7997b20f5f5e7ab29d07c2
b3f3e066e03c3af32b607e16083a7c1c9ca6bb82423de27d41bf12513c20f16d
O=C1C[C@H](COCc2ccccc2)[C@@H](c2ccccc2)C1
C-[OH;D1;+0:1].C=[C;H0;D3;+0:2]1-[C:3]-[C:4]-[C:5]-[C:6]-1>>[O;H0;D1;+0:1]=[C;H0;D3;+0:2]1-[C:3]-[C:4]-[C:5]-[C:6]-1
null
[]
null
null
10
MINUTE
A solution of 1-(S)-benzyloxymethyl-2-(S)-(3-fluorophenyl)-4-methylenecyclopentane from Step A (7.1 g, 25.5 mmol) in methanol (300 mL) was cooled in a dry ice/acetone bath and ozone was bubbled into the solution until the blue color persisted. The excess ozone was removed with a stream of nitrogen and then dimethylsulf...
10.6084/m9.figshare.5104873.v1
null
Vinyl.Methanol
Ketone
C1CCCC1
C1CCCC1
C1CCCC1.c1ccccc1.c1ccccc1
Other
null
null
0.166667
C=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1.CO>>O=C1C[C@H](COCc2ccccc2)[C@@H](c2cccc(F)c2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e9a34e53b9a1434693a6a7c389a733f1
COC(OC)N(C)C.O=C(Cc1ccc(Cl)cc1)c1ccc(Cl)cc1Cl>>CN(C)C=C(C(=O)c1ccc(Cl)cc1Cl)c1ccc(Cl)cc1
ClC1=C(C=CC(=C1)Cl)C(=O)CC1=CC=C(C=C1)Cl.COC(N(C)C)OC>>CN(C=C(C(=O)C1=C(C=C(C=C1)Cl)Cl)C1=CC=C(C=C1)Cl)C
CO[CH:4](OC)[N:2]([CH3:1])[CH3:3].[CH2:5]([C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([Cl:12])[cH:13][c:14]1[Cl:15])[c:16]1[cH:17][cH:18][c:19]([Cl:20])[cH:21][cH:22]1>>[CH3:1][N:2]([CH3:3])[CH:4]=[C:5]([C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([Cl:12])[cH:13][c:14]1[Cl:15])[c:16]1[cH:17][cH:18][c:19]([Cl:20])[cH:21][cH:22]1
COC(OC)N(C)C.O=C(Cc1ccc(Cl)cc1)c1ccc(Cl)cc1Cl
CN(C)C=C(C(=O)c1ccc(Cl)cc1Cl)c1ccc(Cl)cc1
null
null
CN(C)C=O
C-C Coupling
OtherReaction
57f48fac7254684faf48980af66a0d538cb8dee0ab05f049059285d4840b8be4
49ae3600e90e05c7cda8811d9438748b91211f407b3eab7b1bcb51e798f4d85a
[CH]=C(C(=O)c1ccccc1)c1ccccc1
C-O-[CH;D3;+0:1](-O-C)-[#7:2](-[C;D1;H3:3])-[C;D1;H3:4].[O;D1;H0:5]=[C:6](-[c:7])-[CH2;D2;+0:8]-[c:9](:[c:10]):[c:11]>>[C;D1;H3:3]-[#7:2](-[C;D1;H3:4])-[CH;D2;+0:1]=[C;H0;D3;+0:8](-[C:6](=[O;D1;H0:5])-[c:7])-[c:9](:[c:10]):[c:11]
null
[]
null
null
null
null
A solution of 4-chlorobenzyl 2,4-dichlorophenyl ketone (4.5 g, 14.4 mmol) and dimethyl-formamide dimethylacetal (7.7 mL, 58 mmol) in DMF (60 mL) was heated at 75° C. for 20 h. The volatiles were removed in vacuo to provide the crude product which was used directly in the next step. HPLC/MS: 354 (M+1), 356 (M+3); Rt=3.4...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ether.Ether
Enamine
null
null
c1ccccc1.c1ccccc1
HO-
CN(C)C=O
null
null
COC(OC)N(C)C.O=C(Cc1ccc(Cl)cc1)c1ccc(Cl)cc1Cl>CN(C)C=O>CN(C)C=C(C(=O)c1ccc(Cl)cc1Cl)c1ccc(Cl)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-69b20dddb4ce4c1fbef670bef6b342b4
CN(C)C=C(C(=O)c1ccc(Cl)cc1Cl)c1ccc(Cl)cc1.N#CCC(N)=O>>N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccc(Cl)cc2Cl)[nH]c1=O
CN(C=C(C(=O)C1=C(C=C(C=C1)Cl)Cl)C1=CC=C(C=C1)Cl)C.C(#N)CC(=O)N.CO.[H-].[Na+]>>ClC1=C(C=CC(=C1)Cl)C1=C(C=C(C(N1)=O)C#N)C1=CC=C(C=C1)Cl
CN(C)[CH:4]=[C:5]([c:6]1[cH:7][cH:8][c:9]([Cl:10])[cH:11][cH:12]1)[C:13](=O)[c:14]1[cH:15][cH:16][c:17]([Cl:18])[cH:19][c:20]1[Cl:21].[N:1]#[C:2][CH2:3][C:23]([NH2:22])=[O:24]>>[N:1]#[C:2][c:3]1[cH:4][c:5](-[c:6]2[cH:7][cH:8][c:9]([Cl:10])[cH:11][cH:12]2)[c:13](-[c:14]2[cH:15][cH:16][c:17]([Cl:18])[cH:19][c:20]2[Cl:21]...
CN(C)C=C(C(=O)c1ccc(Cl)cc1Cl)c1ccc(Cl)cc1.N#CCC(N)=O
N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccc(Cl)cc2Cl)[nH]c1=O
null
null
CN(C)C=O
Aromatic Heterocycle Formation
OtherReaction
60e6cdceb0baa245fe4412e5afd8e8b3b5ab470991e8279dcbe754fb697cedb2
9bf1fd3c6bd3248cd0029464a9f1478a19f5ad042fa396153933395993aab801
O=c1ccc(-c2ccccc2)c(-c2ccccc2)[nH]1
C-N(-C)-[CH;D2;+0:1]=[C;H0;D3;+0:2](-[C;H0;D3;+0:3](=O)-[c;H0;D3;+0:4](:[c:5]:[c:6]):[c:7](-[Cl;D1;H0:8]):[c:9])-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14].[N;D1;H0:15]#[C:16]-[CH2;D2;+0:17]-[C;H0;D3;+0:18](-[NH2;D1;+0:19])=[O;D1;H0:20]>>[Cl;D1;H0:8]-[c:7](:[c:9]):[c;H0;D3;+0:4](-[c;H0;D3;+0:3]1:[nH;D2;+0:19]:[c;H0;...
null
[]
95
CELSIUS
null
null
A solution of 3-dimethylamino-1-(2,4-dichlorophenyl)-2-(4-chlorophenyl)prop-2-en-1-one (14.4 mmol assumed) from Step A, cyanoacetamide (1.33 g, 15.8 mmol), and methanol (1.3 mL, 32 mmol) in DMF (35 mL) was added dropwise to a suspension of sodium hydride (60% in mineral oil) (1.45 g, 36 mmol) in DMF (16 mL) at rt. Afte...
10.6084/m9.figshare.5104873.v1
null
Enamine.Ketone.Primary amide
null
null
c1cnccc1
c1cnccc1.c1ccccc1.c1ccccc1
HO-
CN(C)C=O
95
null
CN(C)C=C(C(=O)c1ccc(Cl)cc1Cl)c1ccc(Cl)cc1.N#CCC(N)=O>CN(C)C=O>N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccc(Cl)cc2Cl)[nH]c1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c15f147adfaa4abe825a35be35b3fb8b
N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccc(Cl)cc2Cl)[nH]c1=O.O=C(CCl)c1ccccc1>>Nc1c(C(=O)c2ccccc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ClC1=C(C=CC(=C1)Cl)C1=C(C=C(C(N1)=O)C#N)C1=CC=C(C=C1)Cl.C([O-])([O-])=O.[Cs+].[Cs+].ClCC(=O)C1=CC=CC=C1>>NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(=O)C2=CC=CC=C2
[N:1]#[C:2][c:33]1[c:13](=[O:12])[nH:14][c:15](-[c:16]2[cH:17][cH:18][c:19]([Cl:20])[cH:21][c:22]2[Cl:23])[c:24](-[c:25]2[cH:26][cH:27][c:28]([Cl:29])[cH:30][cH:31]2)[cH:32]1.Cl[CH2:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1>>[NH2:1][c:2]1[c:3]([C:4](=[O:5])[c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[o:12][c:1...
N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccc(Cl)cc2Cl)[nH]c1=O.O=C(CCl)c1ccccc1
Nc1c(C(=O)c2ccccc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
null
Aromatic Heterocycle Formation
OtherReaction
1c3dde6f8fb234f99de372746776db1852e1e639963c229bf01260e389d5e88d
481fee288c2b1a3101ebae707e584a0e925bd48483299d9da5a41b1420634672
O=C(c1ccccc1)c1cc2cc(-c3ccccc3)c(-c3ccccc3)nc2o1
Cl-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[c:10](-[c:11]):[nH;D2;+0:12]:[c;H0;D3;+0:13]:1=[O;H0;D1;+0:14]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[c:10](-[c:11]):[n;H0;D2;+0:12]:[c;H0;D3;+0:13]:2:[o;H0;D2;+0:14]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
16
HOUR
A solution of the product from Step B (0.300 g; 0.8 mmol) in DMP (8 mL) was treated with cesium carbonate (0.521 g; 1.6 mmol), 2-chloroacetophenone (0.124 g; 0.8 mmol), and stirred at room temperature for 16 hours. The reaction mixture was partitioned between ethyl acetate and saturated NaHCO3 solution. The organic lay...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Nitrile
Ketone.Primary amine
c1cnccc1
c1cnc2occc2c1
c1ccccc1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
null
null
16
N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccc(Cl)cc2Cl)[nH]c1=O.O=C(CCl)c1ccccc1>>Nc1c(C(=O)c2ccccc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7e87674c3aba466295873e89f7a3ec9d
CC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>>CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ClC1=CC=C(C=C1)C=1C(=NC(=C(C#N)C1)OCC(C)=O)C1=C(C=C(C=C1)Cl)Cl.[O-]CC.[Na+]>>NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C)=O
[CH3:1][C:2](=[O:3])[CH2:4][O:5][c:6]1[n:7][c:8](-[c:9]2[cH:10][cH:11][c:12]([Cl:13])[cH:14][c:15]2[Cl:16])[c:17](-[c:18]2[cH:19][cH:20][c:21]([Cl:22])[cH:23][cH:24]2)[cH:25][c:26]1[C:27]#[N:28]>>[CH3:1][C:2](=[O:3])[c:4]1[o:5][c:6]2[n:7][c:8](-[c:9]3[cH:10][cH:11][c:12]([Cl:13])[cH:14][c:15]3[Cl:16])[c:17](-[c:18]3[cH...
CC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N
CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
afeb9d0652c7b91e28d2fc40e15810604a7053aaa837e966d0d1156989738b30
115ab1fe56a5ae93cee071ae15ca2fbb717f63761b06155835b0712a0ef50301
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
[C;D1;H3:1]-[C:2](=[O;D1;H0:3])-[CH2;D2;+0:4]-[O;H0;D2;+0:5]-[c:6](:[#7;a:7]:[c:8]):[c:9](-[C;H0;D2;+0:10]#[N;H0;D1;+0:11]):[c:12]>>[C;D1;H3:1]-[C:2](=[O;D1;H0:3])-[c;H0;D3;+0:4]1:[o;H0;D2;+0:5]:[c:6](:[#7;a:7]:[c:8]):[c:9](:[c:12]):[c;H0;D3;+0:10]:1-[NH2;D1;+0:11]
null
[]
null
null
null
null
A solution of the product from Step A (0.126 g; 0.292 mmol) in ethanol (4 mL) was treated with sodium ethoxide (0.040 g; 0.584 mmol) and stirred at reflux for 1 hour. The reaction was allowed to cool to room temperature and quenched with saturated NaHCO3 solution. The reaction mixture was partitioned between ethyl acet...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ether.Nitrile
Ketone.Primary amine
c1ccncc1
c1cnc2occc2c1
c1cnc2occc2c1.c1ccccc1.c1ccccc1
null
C(C)O
null
null
CC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>C(C)O>CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8c635e54935543898c0a9c00395ecef1
CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CCN(CC)CC.CS(=O)(=O)Cl>>CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N(S(C)(=O)=O)S(C)(=O)=O
NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C)=O.CS(=O)(=O)Cl.C(C)N(CC)CC>>C(C)(=O)C1=C(C=2C(=NC(=C(C2)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)O1)N(S(=O)(=O)C)S(=O)(=O)C
[CH3:1][C:2](=[O:3])[c:4]1[o:5][c:6]2[n:7][c:8](-[c:9]3[cH:10][cH:11][c:12]([Cl:13])[cH:14][c:15]3[Cl:16])[c:17](-[c:18]3[cH:19][cH:20][c:21]([Cl:22])[cH:23][cH:24]3)[cH:25][c:26]2[c:27]1[NH2:28].CCN(CC)C[CH3:34].Cl[S:29]([CH3:30])(=[O:31])=[O:32]>>[CH3:1][C:2](=[O:3])[c:4]1[o:5][c:6]2[n:7][c:8](-[c:9]3[cH:10][cH:11][c...
CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CCN(CC)CC.CS(=O)(=O)Cl
CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N(S(C)(=O)=O)S(C)(=O)=O
null
null
C(Cl)Cl
Oxidation
OtherReaction
28dc40e546c6cce7c71516552b4ad9521de3a79d04e582ba1e6a06d57c835550
2bb3125db569d4a0c90efcb3ae96ba2c88b9226c575694149f023fc9ffefbf6e
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
C-C-N(-C-C)-C-[CH3;D1;+0:1].Cl-[S;H0;D4;+0:2](-[C;D1;H3:3])(=[O;D1;H0:4])=[O;D1;H0:5].[#7;a:6]:[c:7]1:[#8;a:8]:[c:9](-[C:10](-[C;D1;H3:11])=[O;D1;H0:12]):[c:13](-[NH2;D1;+0:14]):[c:15]:1>>[#7;a:6]:[c:7]1:[#8;a:8]:[c:9](-[C:10](-[C;D1;H3:11])=[O;D1;H0:12]):[c:13](-[N;H0;D3;+0:14](-[#16:16](-[CH3;D1;+0:1])(=[O;D1;H0:17])...
null
[]
null
null
2
HOUR
A solution of 0.030 g (0.0696 mmol)of the product from Example 5 in CH2Cl2 (1 mL) cooled to 0° C. was treated with methanesulfonyl chloride (5 μL; 0.0696 mmol), followed by triethylamine (30 μL; 0.209 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 2 h. The reaction was quenched with...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Tertiary amine.Sulfonyl halide
Tertiary amine
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
C(Cl)Cl
null
2
CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CCN(CC)CC.CS(=O)(=O)Cl>C(Cl)Cl>CC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N(S(C)(=O)=O)S(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1e05681d149548b4b3f14d7ef43684ef
CCOC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>>CCOC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N
NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(=O)OCC.C(CO)(=O)OCC.C([O-])([O-])=O.[Cs+].[Cs+]>>ClC1=CC=C(C=C1)C=1C=C(C(=NC1C1=C(C=C(C=C1)Cl)Cl)OCC(=O)OCC)C#N
[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[o:7][c:8]2[n:9][c:10](-[c:11]3[cH:12][cH:13][c:14]([Cl:15])[cH:16][c:17]3[Cl:18])[c:19](-[c:20]3[cH:21][cH:22][c:23]([Cl:24])[cH:25][cH:26]3)[cH:27][c:28]2[c:29]1[NH2:30]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][O:7][c:8]1[n:9][c:10](-[c:11]2[cH:12][cH:13][c:14]([Cl:15])[cH:16][c:...
CCOC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
CCOC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N
null
null
C1(=CC=CC=C1)C
Miscellaneous
OtherReaction
c98c0adc09f6bda89fb656a6801ef398ca5e5ec0ef38903eb4c87a6f73f10b53
d3ecc5cca77061b45721069d4e9a17b24829facb7c096d498f145e2b57bd7226
c1ccc(-c2cccnc2-c2ccccc2)cc1
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[c;H0;D3;+0:5]1:[o;H0;D2;+0:6]:[c:7](:[#7;a:8]:[c:9]):[c:10](:[c:11]):[c;H0;D3;+0:12]:1-[NH2;D1;+0:13]>>[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH2;D2;+0:5]-[O;H0;D2;+0:6]-[c:7](:[#7;a:8]:[c:9]):[c:10](-[C;H0;D2;+0:12]#[N;H0;D1;+0:13]):[c:11]
null
[]
80
CELSIUS
6
HOUR
A solution of 1.55 g (3.93 mmol) of the product from Step A in toluene (20 mL) was treated with ethyl glycolate (0.41 mL; 4.33 mmol) and cesium carbonate (2.54 g; 7.8 mmol). The reaction mixture was heated in a sealed pressure tube at 80° C. and stirred for 6 h. The reaction mixture was cooled to room temperature and p...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Ester.Ether.Nitrile
c1cnc2occc2c1
c1ccncc1
c1ccncc1.c1ccccc1.c1ccccc1
null
C1(=CC=CC=C1)C
80
6
CCOC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>C1(=CC=CC=C1)C>CCOC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-18a54a893318434ebd0c2f0f966da44b
CCOC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>>CCOC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
C[Si](C)(C)[N-][Si](C)(C)C.[Li+].ClC1=CC=C(C=C1)C=1C=C(C(=NC1C1=C(C=C(C=C1)Cl)Cl)OCC(=O)OCC)C#N>>NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][O:7][c:8]1[n:9][c:10](-[c:11]2[cH:12][cH:13][c:14]([Cl:15])[cH:16][c:17]2[Cl:18])[c:19](-[c:20]2[cH:21][cH:22][c:23]([Cl:24])[cH:25][cH:26]2)[cH:27][c:28]1[C:29]#[N:30]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[o:7][c:8]2[n:9][c:10](-[c:11]3[cH:12][cH:13][c:14]([Cl:15])[cH:16][c:17...
CCOC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N
CCOC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
null
null
C1CCOC1
Aromatic Heterocycle Formation
OtherReaction
59bcb1d0292a9d6aab4c779dc11fad7b9f43062efa223c362ac1ee6a27f4c785
9dcfc7fb45090136d7ea5d1e73f2fc7bd6ce09ea58bac801b2d4160abff5cb53
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH2;D2;+0:5]-[O;H0;D2;+0:6]-[c:7](:[#7;a:8]:[c:9]):[c:10](-[C;H0;D2;+0:11]#[N;H0;D1;+0:12]):[c:13]>>[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[c;H0;D3;+0:5]1:[o;H0;D2;+0:6]:[c:7](:[#7;a:8]:[c:9]):[c:10](:[c:13]):[c;H0;D3;+0:11]:1-[NH2;D1;+0:12]
null
[]
0
CELSIUS
30
MINUTE
A solution of the product from Step B (0.130 g; 0.282 mmol) in THF (3 mL) cooled to 0° C. was treated with 1 M solution of lithium bis(trimethylsilyl)amide in THF (0.85 mL; 0.85 mmol) and stirred at 0° C. under nitrogen for 30 minutes. The reaction mixture was quenched at 0° C. with 10% aqueous NaHSO4 solution. The rea...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether.Nitrile
Ester.Primary amine
c1ccncc1
c1cnc2occc2c1
c1cnc2occc2c1.c1ccccc1.c1ccccc1
null
C1CCOC1
0
0.5
CCOC(=O)COc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>C1CCOC1>CCOC(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cb04649c7f1948398453cc6289ed3098
O=C(c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F)N1CCCCC1>>Nc1c(C(=O)N2CCCCC2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2NC(C(F)(F)F)=O)C(=O)N2CCCCC2.C(=O)([O-])[O-].[K+].[K+]>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2N)C(=O)N2CCCCC2
O=C(C(F)(F)F)[NH:1][c:2]1[c:3]([C:4](=[O:5])[N:6]2[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]2)[o:12][c:13]2[n:14][c:15](-[c:16]3[cH:17][cH:18][c:19]([Cl:20])[cH:21][c:22]3[Cl:23])[c:24](-[c:25]3[cH:26][cH:27][c:28]([Cl:29])[cH:30][cH:31]3)[cH:32][c:33]12>>[NH2:1][c:2]1[c:3]([C:4](=[O:5])[N:6]2[CH2:7][CH2:8][CH2:9][CH2:10][C...
O=C(c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F)N1CCCCC1
Nc1c(C(=O)N2CCCCC2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
CO
Reduction
Hydrogenolysis of amides/imides/carbamates
44b36597c7daf0608965c52c8db8a9220c21d9447ce54e0af375898475f3493f
caaeb83af2cb178156ae90fe7f610a106cd4bb5397d23f56d37a7fe11e2668ed
O=C(c1cc2cc(-c3ccccc3)c(-c3ccccc3)nc2o1)N1CCCCC1
F-C(-F)(-F)-C(=O)-[NH;D2;+0:1]-[c:2]1:[c:3]:[c:4](:[#7;a:5]):[#8;a:6]:[c:7]:1-[C:8](-[#7:9])=[O;D1;H0:10]>>[#7:9]-[C:8](=[O;D1;H0:10])-[c:7]1:[#8;a:6]:[c:4](:[#7;a:5]):[c:3]:[c:2]:1-[NH2;D1;+0:1]
null
[]
null
null
null
null
A solution of 35 mg of the product of Example 12 dissolved in 1 mL of methanol was treated with 41 mg of K2CO3 at 60° C. for 2 hours. The reaction mixture was then partitioned between EtOAc and water and the organic product was extracted. The extracts were dried (Na2SO4), filtered and evaporated in vacuo to afford to a...
10.6084/m9.figshare.5104873.v1
null
Trifluoro group.Secondary amide
Primary amine
null
null
C1CC[NH]CC1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
Other
CO
null
null
O=C(c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F)N1CCCCC1>CO>Nc1c(C(=O)N2CCCCC2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-abf83597ba6e4559a8be72219905d54c
CC(=O)Cl.CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>>CC(=O)Nc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
C(C)N(CC)CC.NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)C)=O.C(C)(=O)Cl>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2NC(C)=O)C(C(C)(C)C)=O
Cl[C:2]([CH3:1])=[O:3].[NH2:4][c:5]1[c:6]([C:7](=[O:8])[C:9]([CH3:10])([CH3:11])[CH3:12])[o:13][c:14]2[n:15][c:16](-[c:17]3[cH:18][cH:19][c:20]([Cl:21])[cH:22][c:23]3[Cl:24])[c:25](-[c:26]3[cH:27][cH:28][c:29]([Cl:30])[cH:31][cH:32]3)[cH:33][c:34]12>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[c:6]([C:7](=[O:8])[C:9]([CH3:10])([C...
CC(=O)Cl.CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
CC(=O)Nc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
Cl-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[#7;a:4]:[c:5]1:[#8;a:6]:[c:7](-[C:8]=[O;D1;H0:9]):[c:10](-[NH2;D1;+0:11]):[c:12]:1>>[#7;a:4]:[c:5]1:[#8;a:6]:[c:7](-[C:8]=[O;D1;H0:9]):[c:10](-[NH;D2;+0:11]-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3]):[c:12]:1
null
[]
null
null
1
HOUR
A solution of 0.050 g (0.106 mmol) of the product from Example 17 in CH2Cl2 (1 mL) at 0° C. was treated with acetyl chloride (8 μL; 0.106 mmol) followed by triethylamine (15 μL; 0.106 mmol). After the addition, the reaction mixture was warmed to RT and stirred for 1 hour. The reaction was quenched with saturated NaHCO3...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
C(Cl)Cl
null
1
CC(=O)Cl.CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>C(Cl)Cl>CC(=O)Nc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d2815f51ce1f4e4fbbb926016cb5c247
CC(C)(C)C(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>CC(C)(C)C(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
C(C)N(CC)CC.NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(=O)C=2C=NC=CC2.CC(C(=O)Cl)(C)C>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2NC(C(C)(C)C)=O)C(=O)C=2C=NC=CC2
Cl[C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])=[O:6].[NH2:7][c:8]1[c:9]([C:10](=[O:11])[c:12]2[cH:13][cH:14][cH:15][n:16][cH:17]2)[o:18][c:19]2[n:20][c:21](-[c:22]3[cH:23][cH:24][c:25]([Cl:26])[cH:27][c:28]3[Cl:29])[c:30](-[c:31]3[cH:32][cH:33][c:34]([Cl:35])[cH:36][cH:37]3)[cH:38][c:39]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[C:5]...
CC(C)(C)C(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
CC(C)(C)C(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
O=C(c1cccnc1)c1cc2cc(-c3ccccc3)c(-c3ccccc3)nc2o1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])(-[C;D1;H3:5])-[C;D1;H3:6].[#7;a:7]:[c:8]1:[#8;a:9]:[c:10](-[C:11]=[O;D1;H0:12]):[c:13](-[NH2;D1;+0:14]):[c:15]:1>>[#7;a:7]:[c:8]1:[#8;a:9]:[c:10](-[C:11]=[O;D1;H0:12]):[c:13](-[NH;D2;+0:14]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])(-[C;D1;H3:5])-[C;D1;H3:6]):[c...
null
[]
null
null
16
HOUR
A solution of 0.200 g (0.405 mmol) of the product from Example 26 in CH2Cl2 (4 mL) at 0° C. was treated with trimethylacetyl chloride (50 μL; 0.405 mmol) followed by triethylamine (113 μL; 0.810 mmol). After the addition, the reaction mixture was warmed to room temperature and stirred for 16 hours. The reaction was que...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccncc1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
C(Cl)Cl
null
16
CC(C)(C)C(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>C(Cl)Cl>CC(C)(C)C(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6b854e7dc2de4f828680e0b9d210b2fe
COC(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>COC(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
C(C)(C)N(CC)C(C)C.NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(=O)C=2C=NC=CC2.ClC(=O)OC>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2NC(OC)=O)C(=O)C=2C=NC=CC2
Cl[C:3]([O:2][CH3:1])=[O:4].[NH2:5][c:6]1[c:7]([C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][n:14][cH:15]2)[o:16][c:17]2[n:18][c:19](-[c:20]3[cH:21][cH:22][c:23]([Cl:24])[cH:25][c:26]3[Cl:27])[c:28](-[c:29]3[cH:30][cH:31][c:32]([Cl:33])[cH:34][cH:35]3)[cH:36][c:37]12>>[CH3:1][O:2][C:3](=[O:4])[NH:5][c:6]1[c:7]([C:8](=[O:9]...
COC(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
COC(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
C(Cl)Cl
Protection
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
038720aa61a7efa0f2a9ee6f2e0adf63a9ffdc2be4697c11a6215baef34f97b2
205f353513ce9506ab61831799da8fb73ec2ef5cfa927664496d3ce72c438860
O=C(c1cccnc1)c1cc2cc(-c3ccccc3)c(-c3ccccc3)nc2o1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4].[#7;a:5]:[c:6]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:11](-[NH2;D1;+0:12]):[c:13]:1>>[#7;a:5]:[c:6]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:11](-[NH;D2;+0:12]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4]):[c:13]:1
null
[]
null
null
16
HOUR
A solution of 0.030 g (0.0607 mmol) of the product from Example 26 in CH2Cl2 (0.6 mL) at 0° C. was treated with methyl chloroformate (5 μL; 0.0607 mmol) followed by diisopropylethylamine (10 μL; 0.0607 mmol). After the addition, the reaction mixture was warmed to room temperature and stirred for 16 hours. The reaction ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether.Primary amine
Carbamic ester
null
null
c1ccncc1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
C(Cl)Cl
null
16
COC(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>C(Cl)Cl>COC(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-465b85b846ba480ab12263322a36681a
CN(C)S(=O)(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>CN(C)C(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
[H-].[Na+].C1CCOC1.NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(=O)C=2C=NC=CC2.C1CCOC1.CN(S(=O)(=O)Cl)C>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2NC(N(C)C)=O)C(=O)C=2C=NC=CC2
O=S(Cl)([N:2]([CH3:1])[CH3:3])=[O:5].[NH2:6][c:7]1[c:8]([C:9](=[O:10])[c:11]2[cH:12][cH:13][cH:14][n:15][cH:16]2)[o:17][c:18]2[n:19][c:20](-[c:21]3[cH:22][cH:23][c:24]([Cl:25])[cH:26][c:27]3[Cl:28])[c:29](-[c:30]3[cH:31][cH:32][c:33]([Cl:34])[cH:35][cH:36]3)[cH:37][c:38]12>>[CH3:1][N:2]([CH3:3])[C:4](=[O:5])[NH:6][c:7]...
CN(C)S(=O)(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
CN(C)C(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
null
Acylation
OtherReaction
6c16e9e6c124c414c1ad4cacebf047406027aae7e5b317e16f63e05e6a23fab2
0759a3c95a8b36ced23f0830233262728dd65cae0539873906a2229ea157808c
O=C(c1cccnc1)c1cc2cc(-c3ccccc3)c(-c3ccccc3)nc2o1
Cl-S(=O)(=[O;H0;D1;+0:1])-[N;H0;D3;+0:2](-[C;D1;H3:3])-[C;D1;H3:4].[#7;a:5]:[c:6]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:11](-[NH2;D1;+0:12]):[c:13]:1>>[#7;a:5]:[c:6]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:11](-[NH;D2;+0:12]-[C:14](=[O;H0;D1;+0:1])-[N;H0;D3;+0:2](-[C;D1;H3:3])-[C;D1;H3:4]):[c:13]:1
null
[]
0
CELSIUS
30
MINUTE
To a suspension of sodium hydride (0.004 g; 60% dispersion; 0.111 mmol) in THF (0.5 mL) at 0° C. was added a solution of 0.050 g 0.101 mmol) of the product from Example 26 (in THF (0.5 mL) and the reaction mixture was stirred at 0° C. for 30 minutes. Dimethylsulfamoyl chloride (9 μL; 0.101 mmol) was added dropwise and ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Tertiary amine
Urea
null
null
c1ccncc1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
null
0
0.5
CN(C)S(=O)(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>CN(C)C(=O)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-670afcfaaaf549ff9091b4ef1486c46e
C1CC2CCC1CN2.CC(=O)Nc1c(C(=O)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>CC(=O)Nc1c(C(=O)N2CC3CCC2CC3)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
C(C)(=O)NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(=O)O.Cl.C12NCC(CC1)CC2.C(CCl)Cl.CN1CCOCC1>>C12N(CC(CC1)CC2)C(=O)C2=C(C=1C(=NC(=C(C1)C1=CC=C(C=C1)Cl)C1=C(C=C(C=C1)Cl)Cl)O2)NC(C)=O
[NH:9]1[CH2:10][CH:11]2[CH2:12][CH2:13][CH:14]1[CH2:15][CH2:16]2.O[C:7]([c:6]1[c:5]([NH:4][C:2]([CH3:1])=[O:3])[c:38]2[c:18]([o:17]1)[n:19][c:20](-[c:21]1[cH:22][cH:23][c:24]([Cl:25])[cH:26][c:27]1[Cl:28])[c:29](-[c:30]1[cH:31][cH:32][c:33]([Cl:34])[cH:35][cH:36]1)[cH:37]2)=[O:8]>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[c:6](...
C1CC2CCC1CN2.CC(=O)Nc1c(C(=O)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
CC(=O)Nc1c(C(=O)N2CC3CCC2CC3)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
CN(C)C=1C=CN=CC1
C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Carboxylic Acids
6a9cf6b8de28dd6c2a4b0ec408de367f03e79e81384ba9bc53d30df5e6067a68
c5e4172490b2731ba9322b68af56376edadc31ce0bb9a3dfdea23a1817a852fd
O=C(c1cc2cc(-c3ccccc3)c(-c3ccccc3)nc2o1)N1CC2CCC1CC2
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#8;a:5]:[c:6]:[#7;a:7].[C:8]-[C:9]-[NH;D2;+0:10]-[C:11](-[C:12])-[C:13]>>[#7;a:7]:[c:6]:[#8;a:5]:[c:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:10](-[C:9]-[C:8])-[C:11](-[C:12])-[C:13]):[c:4]
null
[]
null
null
16
HOUR
A solution of 0.027 g (0.0568 mmol) of the product from Step A in CH2Cl2 (0.6 mL) was treated with 2-azabicyclo[2.2.2]octane hydrochloride (0.009 g; 0.0625 mmol), EDC (0.016 g; 0.0852 mmol), DMAP (0.007 g; 0.0568 mmol), and 1-methylmorpholine (19 μL; 0.170 mmol), then stirred at room temperature for 16 hours. The react...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Tertiary amide
C1CC2CCC1CN2
C1CC2CCC1C[NH]2
c1cnc2occc2c1.c1ccccc1.c1ccccc1.C1CC2CCC1C[NH]2
HO-
CN(C)C=1C=CN=CC1.C(Cl)Cl
null
16
C1CC2CCC1CN2.CC(=O)Nc1c(C(=O)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>CN(C)C=1C=CN=CC1.C(Cl)Cl>CC(=O)Nc1c(C(=O)N2CC3CCC2CC3)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-679402d1219b469b81cbcf32fa23699d
CN(C(=O)C(F)(F)F)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>CNc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2N(C(C(F)(F)F)=O)C)C(C(C)(C)C)=O.C([O-])([O-])=O.[K+].[K+]>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2NC)C(C(C)(C)C)=O
O=C(C(F)(F)F)[N:2]([CH3:1])[c:3]1[c:4]([C:5](=[O:6])[C:7]([CH3:8])([CH3:9])[CH3:10])[o:11][c:12]2[n:13][c:14](-[c:15]3[cH:16][cH:17][c:18]([Cl:19])[cH:20][c:21]3[Cl:22])[c:23](-[c:24]3[cH:25][cH:26][c:27]([Cl:28])[cH:29][cH:30]3)[cH:31][c:32]12>>[CH3:1][NH:2][c:3]1[c:4]([C:5](=[O:6])[C:7]([CH3:8])([CH3:9])[CH3:10])[o:1...
CN(C(=O)C(F)(F)F)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
CNc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
CO.O
Reduction
Hydrogenolysis of tertiary amines
16961a3d99942c0ab361f2149cf4766848c112f4d4d9e5e515a20194fa44ecb0
9d0759623d33e2d41aafe1af3bb1025d4d7a88f20060c872279b889c110cab65
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
F-C(-F)(-F)-C(=O)-[N;H0;D3;+0:1](-[C;D1;H3:2])-[c:3]1:[c:4]:[c:5](:[#7;a:6]):[#8;a:7]:[c:8]:1-[C:9]=[O;D1;H0:10]>>[#7;a:6]:[c:5]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:3](-[NH;D2;+0:1]-[C;D1;H3:2]):[c:4]:1
null
[]
null
null
null
null
A solution of the product from Step A (0.0703 mmol) in methanol (2 mL) and water (0.1 mL) was treated with potassium carbonate (0.049 g; 0.351 mmol) at room temperature. The reaction mixture was stirred a room temperature until the reaction was judged complete by TLC analysis. The reaction mixture was then partitioned ...
10.6084/m9.figshare.5104873.v1
null
Trifluoro group.Tertiary amide
Secondary amine
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
Other
CO.O
null
null
CN(C(=O)C(F)(F)F)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>CO.O>CNc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f3e770690d984187be9a3bc66ad344d0
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CI.CN(C)C=O>>CN(C)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
IC.NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)C)=O.[H-].[Na+].CN(C)C=O>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2N(C)C)C(C(C)(C)C)=O
[NH2:2][c:4]1[c:5]([C:6](=[O:7])[C:8]([CH3:9])([CH3:10])[CH3:11])[o:12][c:13]2[n:14][c:15](-[c:16]3[cH:17][cH:18][c:19]([Cl:20])[cH:21][c:22]3[Cl:23])[c:24](-[c:25]3[cH:26][cH:27][c:28]([Cl:29])[cH:30][cH:31]3)[cH:32][c:33]12.I[CH3:1].CN(C=O)[CH3:3]>>[CH3:1][N:2]([CH3:3])[c:4]1[c:5]([C:6](=[O:7])[C:8]([CH3:9])([CH3:10]...
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CI.CN(C)C=O
CN(C)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
49e97dc5c4663bf1af5b9459b20429dc1c61d967c03ec2264af690226d29471e
6e9cf66e5c33b8adfc96ab6ca734f2e68e464a4b02d1a8813c05c370f4bc819a
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
C-N(-[CH3;D1;+0:1])-C=O.I-[CH3;D1;+0:2].[#7;a:3]:[c:4]1:[#8;a:5]:[c:6](-[C:7]=[O;D1;H0:8]):[c:9](-[NH2;D1;+0:10]):[c:11]:1>>[#7;a:3]:[c:4]1:[#8;a:5]:[c:6](-[C:7]=[O;D1;H0:8]):[c:9](-[N;H0;D3;+0:10](-[CH3;D1;+0:2])-[CH3;D1;+0:1]):[c:11]:1
null
[]
0
CELSIUS
20
MINUTE
A solution of 0.050 g (0.106 mmol) of the product from Example 17 in DMF (1 mL) at 0° C. was treated with sodium hydride (0.010 g; 60% dispersion; 0.232 mmol). After the addition, the reaction mixture was stirred for 20 minutes at 0° C., and then treated with iodomethane (26 μL; 0.424 mmol). The reaction was warmed to ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Primary amine
Tertiary amine
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HI
null
0
0.333333
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CI.CN(C)C=O>>CN(C)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9ab14d756ba14936bc6b2f503da78bc2
CI.CN(C)C=O.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>CN(C)c1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
IC.NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(=O)C=2C=NC=CC2.[H-].[Na+].CN(C)C=O>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2N(C)C)C(=O)C=2C=NC=CC2
I[CH3:1].CN(C=O)[CH3:3].[NH2:2][c:4]1[c:5]([C:6](=[O:7])[c:8]2[cH:9][cH:10][cH:11][n:12][cH:13]2)[o:14][c:15]2[n:16][c:17](-[c:18]3[cH:19][cH:20][c:21]([Cl:22])[cH:23][c:24]3[Cl:25])[c:26](-[c:27]3[cH:28][cH:29][c:30]([Cl:31])[cH:32][cH:33]3)[cH:34][c:35]12>>[CH3:1][N:2]([CH3:3])[c:4]1[c:5]([C:6](=[O:7])[c:8]2[cH:9][cH...
CI.CN(C)C=O.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
CN(C)c1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
49e97dc5c4663bf1af5b9459b20429dc1c61d967c03ec2264af690226d29471e
6e9cf66e5c33b8adfc96ab6ca734f2e68e464a4b02d1a8813c05c370f4bc819a
O=C(c1cccnc1)c1cc2cc(-c3ccccc3)c(-c3ccccc3)nc2o1
C-N(-[CH3;D1;+0:1])-C=O.I-[CH3;D1;+0:2].[#7;a:3]:[c:4]1:[#8;a:5]:[c:6](-[C:7]=[O;D1;H0:8]):[c:9](-[NH2;D1;+0:10]):[c:11]:1>>[#7;a:3]:[c:4]1:[#8;a:5]:[c:6](-[C:7]=[O;D1;H0:8]):[c:9](-[N;H0;D3;+0:10](-[CH3;D1;+0:2])-[CH3;D1;+0:1]):[c:11]:1
null
[]
0
CELSIUS
20
MINUTE
A solution of 0.050 g (0.101 mmol) of the product from Example 26 in DMF (1 mL) at 0° C. was treated with sodium hydride (0.008 g; 60% dispersion; 0.213 mmol). After the addition, the reaction mixture was stirred for 20 minutes at 0° C., and then treated with iodomethane (19 μL; 0.303 mmol). The reaction was warmed to ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Primary amine
Tertiary amine
null
null
c1ccncc1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HI
null
0
0.333333
CI.CN(C)C=O.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>CN(C)c1c(C(=O)c2cccnc2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-537916f9a3f54e7cb12f121d01c3fc54
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CCBr>>CCNc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)C)=O.C(C)Br>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2NCC)C(C(C)(C)C)=O
[NH2:3][c:4]1[c:5]([C:6](=[O:7])[C:8]([CH3:9])([CH3:10])[CH3:11])[o:12][c:13]2[n:14][c:15](-[c:16]3[cH:17][cH:18][c:19]([Cl:20])[cH:21][c:22]3[Cl:23])[c:24](-[c:25]3[cH:26][cH:27][c:28]([Cl:29])[cH:30][cH:31]3)[cH:32][c:33]12.Br[CH2:2][CH3:1]>>[CH3:1][CH2:2][NH:3][c:4]1[c:5]([C:6](=[O:7])[C:8]([CH3:9])([CH3:10])[CH3:11...
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CCBr
CCNc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
fc19a1445ff204e66e51735d0191465bda3c6691fd233624a54742c9d4828411
0b1d32f56ad00f1e5bdae9390f9227bbea012fa2f8203aac34726b8a6761cc7c
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
Br-[CH2;D2;+0:1]-[C;D1;H3:2].[#7;a:3]:[c:4]1:[#8;a:5]:[c:6](-[C:7]=[O;D1;H0:8]):[c:9](-[NH2;D1;+0:10]):[c:11]:1>>[#7;a:3]:[c:4]1:[#8;a:5]:[c:6](-[C:7]=[O;D1;H0:8]):[c:9](-[NH;D2;+0:10]-[CH2;D2;+0:1]-[C;D1;H3:2]):[c:11]:1
null
[]
null
null
null
null
Using the procedure described in Example 39, the product of Example 17 was reacted with one equivalent of ethyl bromide to afford the title compound. HPLC/MS: 500.9 (M+1), 502.9 (M+3); Rt=4.08 min. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary amine
Secondary amine
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HBr
null
null
null
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.CCBr>>CCNc1c(C(=O)C(C)(C)C)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b22fb182a5a04572853f4b28447fe852
N#CCOc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>>N#Cc1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ClC1=CC=C(C=C1)C=1C(=NC(=C(C#N)C1)OCC#N)C1=C(C=C(C=C1)Cl)Cl.C[Si](C)(C)[N-][Si](C)(C)C.[Li+].C1CCOC1>>NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C#N
[N:1]#[C:2][CH2:3][O:4][c:5]1[n:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([Cl:12])[cH:13][c:14]2[Cl:15])[c:16](-[c:17]2[cH:18][cH:19][c:20]([Cl:21])[cH:22][cH:23]2)[cH:24][c:25]1[C:26]#[N:27]>>[N:1]#[C:2][c:3]1[o:4][c:5]2[n:6][c:7](-[c:8]3[cH:9][cH:10][c:11]([Cl:12])[cH:13][c:14]3[Cl:15])[c:16](-[c:17]3[cH:18][cH:19][c:20]([C...
N#CCOc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N
N#Cc1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
null
null
null
Aromatic Heterocycle Formation
OtherReaction
310e82a1a04ad8be5cc811c019c822a32b44ad18376ea0176a8296685624b50f
1840d341887117642bffcff327c44a81dcd63e1f29237a5b99bb06120b967248
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
[N;D1;H0:1]#[C:2]-[CH2;D2;+0:3]-[O;H0;D2;+0:4]-[c:5](:[#7;a:6]:[c:7]):[c:8](-[C;H0;D2;+0:9]#[N;H0;D1;+0:10]):[c:11]>>[N;D1;H0:1]#[C:2]-[c;H0;D3;+0:3]1:[o;H0;D2;+0:4]:[c:5](:[#7;a:6]:[c:7]):[c:8](:[c:11]):[c;H0;D3;+0:9]:1-[NH2;D1;+0:10]
null
[]
0
CELSIUS
15
MINUTE
A solution of the product from Step A (0.132 g; 0.319 mmol) in TB (3 mL) cooled to 0° C. was treated with 1 M solution of lithium bis(trimethylsilyl)amide in THF (701 μL; 0.701 mmol) and stirred at 0° C. under nitrogen for 15 minutes. The reaction mixture was warmed to room temperature and then stirred for an additiona...
10.6084/m9.figshare.5104873.v1
null
Ether.Nitrile
Primary amine
c1ccncc1
c1cnc2occc2c1
c1cnc2occc2c1.c1ccccc1.c1ccccc1
null
null
0
0.25
N#CCOc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>>N#Cc1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f47096e8f5d1498496da5e56b2bf7d62
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.O=C(Cl)CCCCl>>CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CCCCl
NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)C)=O.ClCCCC(=O)Cl.C(C)N(CC)CC>>ClCCCC(=O)NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[c:7]1[o:8][c:9]2[n:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([Cl:16])[cH:17][c:18]3[Cl:19])[c:20](-[c:21]3[cH:22][cH:23][c:24]([Cl:25])[cH:26][cH:27]3)[cH:28][c:29]2[c:30]1[NH2:31].Cl[C:32](=[O:33])[CH2:34][CH2:35][CH2:36][Cl:37]>>[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[c:7]...
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.O=C(Cl)CCCCl
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CCCCl
null
null
C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[#7;a:5]:[c:6]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:11](-[NH2;D1;+0:12]):[c:13]:1>>[#7;a:5]:[c:6]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:11](-[NH;D2;+0:12]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]):[c:13]:1
null
[]
null
null
1.5
HOUR
To a magnetically stirred solution of 0.300 g (0.63 mmol) of the product of Example 17 in 6 mL of CH2Cl2 at 0° C. was added 70 μL (0.63 mmol) of 4-chlorobutyryl chloride and 96 mg (0.95 mmol) of triethylamine. The reaction was stirred for 1.5 h and allowed to warm to room temperature. The reaction mixture was then part...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
C(Cl)Cl
null
1.5
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N.O=C(Cl)CCCCl>C(Cl)Cl>CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CCCCl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-06ce1654413a4001b8df472ef7bcb703
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CCCCl>>CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N1CCCC1=O
[H-].[Na+].ClCCCC(=O)NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)C)=O>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2N2C(CCC2)=O)C(C(C)(C)C)=O
Cl[CH2:32][CH2:33][CH2:34][C:35]([NH:31][c:30]1[c:7]([C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])=[O:6])[o:8][c:9]2[n:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([Cl:16])[cH:17][c:18]3[Cl:19])[c:20](-[c:21]3[cH:22][cH:23][c:24]([Cl:25])[cH:26][cH:27]3)[cH:28][c:29]21)=[O:36]>>[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[c:7]1[o:8][...
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CCCCl
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N1CCCC1=O
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
62f43057f012567ee0d9bea97538013537b046013f70e56d5406a05691c3dc0d
4a6c1e88c9e8bed487b746792f88d478ff36cc235f9a217d4632e6babdebdc9a
O=C1CCCN1c1coc2nc(-c3ccccc3)c(-c3ccccc3)cc12
Cl-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4](=[O;D1;H0:5])-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9](:[#7;a:10]):[#8;a:11]:[c:12]:1-[C:13]=[O;D1;H0:14]>>[#7;a:10]:[c:9]1:[#8;a:11]:[c:12](-[C:13]=[O;D1;H0:14]):[c:7](-[N;H0;D3;+0:6]2-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]-2=[O;D1;H0:5]):[c:8]:1
null
[]
60
CELSIUS
null
null
To a magnetically stirred suspension of 7 mg (0.173 mmol) of sodium hydride in 1 mL THF was slowly added 0.100 g (0.173 mmol) of the product of Example 47 dissolved in 1 mL of THF. After 15 min the addition was complete and the reaction mixture was stirred and heated to 60° C. for 3.5 h. The reaction was then cooled to...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amide
Tertiary amide
null
C1CC[NH]C1
c1cnc2occc2c1.c1ccccc1.c1ccccc1.C1CC[NH]C1
HCl
C1CCOC1
60
null
CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CCCCl>C1CCOC1>CC(C)(C)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N1CCCC1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9b9d55aab8b243c5a6fc73781db5ccd2
CC(=O)OCC(=O)Cl.CC(C)(O)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>>CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)O)=O.C(C)(=O)OCC(=O)Cl.C(C)#N>>C(C)(=O)OCC(=O)NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)O)=O
Cl[C:6]([CH2:5][O:4][C:2]([CH3:1])=[O:3])=[O:7].[NH2:8][c:9]1[c:10]([C:11](=[O:12])[C:13]([CH3:14])([CH3:15])[OH:16])[o:17][c:18]2[n:19][c:20](-[c:21]3[cH:22][cH:23][c:24]([Cl:25])[cH:26][c:27]3[Cl:28])[c:29](-[c:30]3[cH:31][cH:32][c:33]([Cl:34])[cH:35][cH:36]3)[cH:37][c:38]12>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][C:6](=[O...
CC(=O)OCC(=O)Cl.CC(C)(O)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
C(C)(=O)OCC
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#8:4]-[C:5](-[C;D1;H3:6])=[O;D1;H0:7].[#7;a:8]:[c:9]1:[#8;a:10]:[c:11](-[C:12]=[O;D1;H0:13]):[c:14](-[NH2;D1;+0:15]):[c:16]:1>>[#7;a:8]:[c:9]1:[#8;a:10]:[c:11](-[C:12]=[O;D1;H0:13]):[c:14](-[NH;D2;+0:15]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#8:4]-[C:5](-[C;D1;H3:6])=[O;D1;H0:7]):[c...
null
[]
null
null
null
null
The product of Step B (0.120 g; 0.253 mmol) and acetoxyacetyl chloride (0.11 mL; 1.01 mmol) were added to 2 mL of acetonitrile and stirred at room temperature. After 50 minutes the reaction mixture was diluted with ethyl acetate and washed two times with aqueous sodium bicarbonate. The organic layer was dried over sodi...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
C(C)(=O)OCC
null
null
CC(=O)OCC(=O)Cl.CC(C)(O)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>C(C)(=O)OCC>CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1d44fccaefc041d68a448a30ecfbc9e3
CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>>CC(C)(O)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CO
[OH-].[Li+].O.C(C)(=O)OCC(=O)NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=C(C=C2)Cl)Cl)C(C(C)(C)O)=O.CO>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2NC(CO)=O)C(C(C)(C)O)=O
CC(=O)[O:35][CH2:34][C:32]([NH:31][c:30]1[c:7]([C:5]([C:2]([CH3:1])([CH3:3])[OH:4])=[O:6])[o:8][c:9]2[n:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([Cl:16])[cH:17][c:18]3[Cl:19])[c:20](-[c:21]3[cH:22][cH:23][c:24]([Cl:25])[cH:26][cH:27]3)[cH:28][c:29]21)=[O:33]>>[CH3:1][C:2]([CH3:3])([OH:4])[C:5](=[O:6])[c:7]1[o:8][c:9]2[n:...
CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
CC(C)(O)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CO
null
null
C1CCOC1
Reduction
Hydrolysis or Hydrogenolysis of Carboxylic Esters or Thioesters
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
C-C(=O)-[O;H0;D2;+0:1]-[C:2]-[C:3](=[O;D1;H0:4])-[#7:5]-[c:6]:[c:7]:[#8;a:8]>>[#8;a:8]:[c:7]:[c:6]-[#7:5]-[C:3](=[O;D1;H0:4])-[C:2]-[OH;D1;+0:1]
null
[]
null
null
null
null
Lithium hydroxide-H2O (0.004 g; 0.174 mmol), the product of Step C (0.100 g; 0.174 mmol), and methanol (0.3 mL) were combined in 2 mL of THF and stirred at room temperature. The reaction was monitored by TLC until complete at which point the reaction was quenched by addition of 0.50 mL of acetic acid. The reaction was ...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HO-
C1CCOC1
null
null
CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12>C1CCOC1>CC(C)(O)C(=O)c1oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-56f0e6a441a9460baf2227bb5042856e
COC(=O)C(Oc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N)c1ccc(F)c(F)c1>>COC(=O)C1(c2ccc(F)c(F)c2)Oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2C1=O
ClC1=CC=C(C=C1)C=1C=C(C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(C(=O)OC)C1=CC(=C(C=C1)F)F)C#N.C1CCOC1.C1CCOC1.C[Si](C)(C)[NH-].C[Si](C)(C)[NH-].[Li+].[Li+]>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(C2=O)(C(=O)OC)C2=CC(=C(C=C2)F)F
N#[C:36][c:35]1[c:15]([O:14][CH:5]([C:3]([O:2][CH3:1])=[O:4])[c:6]2[cH:7][cH:8][c:9]([F:10])[c:11]([F:12])[cH:13]2)[n:16][c:17](-[c:18]2[cH:19][cH:20][c:21]([Cl:22])[cH:23][c:24]2[Cl:25])[c:26](-[c:27]2[cH:28][cH:29][c:30]([Cl:31])[cH:32][cH:33]2)[cH:34]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([c:6]2[cH:7][cH:8][c:9]([F:10])...
COC(=O)C(Oc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N)c1ccc(F)c(F)c1
COC(=O)C1(c2ccc(F)c(F)c2)Oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2C1=O
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
0d978b6e4b9400ed54bef533c5e070747a1a63797d169cd81c7d0830df3f18b2
6372e17458037521a28318b54428d2d0705ec274dc001be8d214e49aaab58744
O=C1c2cc(-c3ccccc3)c(-c3ccccc3)nc2OC1c1ccccc1
N#[C;H0;D2;+0:1]-[c:2](:[c:3]):[c:4](-[#8:5]-[CH;D3;+0:6](-[C:7](=[O;D1;H0:8])-[#8:9]-[C;D1;H3:10])-[c:11](:[c:12]):[c:13]):[#7;a:14]:[c:15]>>[C;D1;H3:10]-[#8:9]-[C:7](=[O;D1;H0:8])-[C;H0;D4;+0:6]1(-[c:11](:[c:12]):[c:13])-[#8:5]-[c:4](:[#7;a:14]:[c:15]):[c:2](:[c:3])-[C;H0;D3;+0:1]-1=[O;D1;H0:16]
null
[]
null
null
30
MINUTE
To a magnetically stirred solution of 1.20 g (2.14 mmol) the product of Step A dissolved in 12 mL of THF was slowly added 3.2 mL of a 1.0 N solution (3.2 mmol) of lithium bis(trimethylsilylamide) in THF at 0° C. The reaction mixture was stirred for 30 min and allowed to warm to room temperature. The reaction mixture wa...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether.Nitrile
Ketone
null
c1cnc2c(c1)CCO2
c1ccccc1.c1cnc2c(c1)CCO2.c1ccccc1.c1ccccc1
null
null
null
0.5
COC(=O)C(Oc1nc(-c2ccc(Cl)cc2Cl)c(-c2ccc(Cl)cc2)cc1C#N)c1ccc(F)c(F)c1>>COC(=O)C1(c2ccc(F)c(F)c2)Oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2C1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5e1c4faac4c241878ca727421cfe449d
COC(=O)C1(c2ccc(F)c(F)c2)Oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2C1=O>>Oc1c(-c2ccc(F)c(F)c2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(C2=O)(C(=O)OC)C2=CC(=C(C=C2)F)F.[BH4-].[Na+]>>ClC1=CC=C(C=C1)C=1C=C2C(=NC1C1=C(C=C(C=C1)Cl)Cl)OC(=C2O)C2=CC(=C(C=C2)F)F
COC(=O)[C:3]1([c:4]2[cH:5][cH:6][c:7]([F:8])[c:9]([F:10])[cH:11]2)[C:2](=[O:1])[c:33]2[c:13]([n:14][c:15](-[c:16]3[cH:17][cH:18][c:19]([Cl:20])[cH:21][c:22]3[Cl:23])[c:24](-[c:25]3[cH:26][cH:27][c:28]([Cl:29])[cH:30][cH:31]3)[cH:32]2)[O:12]1>>[OH:1][c:2]1[c:3](-[c:4]2[cH:5][cH:6][c:7]([F:8])[c:9]([F:10])[cH:11]2)[o:12]...
COC(=O)C1(c2ccc(F)c(F)c2)Oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2C1=O
Oc1c(-c2ccc(F)c(F)c2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
CCO
Functional Group Interconversion
OtherReaction
4b4af184adbfc9512d460afa65e86656b8968d40567dc72a215f915700b1b99e
73948743e2b7cc73319dbdc34494386c440f48774dd498a1deddf56bb0ad34ec
c1ccc(-c2cc3cc(-c4ccccc4)c(-c4ccccc4)nc3o2)cc1
C-O-C(=O)-[C;H0;D4;+0:1]1(-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5]:[c:6])-[O;H0;D2;+0:7]-[c:8](:[#7;a:9]:[c:10]):[c:11](:[c:12])-[C;H0;D3;+0:13]-1=[O;H0;D1;+0:14]>>[OH;D1;+0:14]-[c;H0;D3;+0:13]1:[c:11](:[c:12]):[c:8](:[#7;a:9]:[c:10]):[o;H0;D2;+0:7]:[c;H0;D3;+0:1]:1-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5]:[c:6]
null
[]
null
null
5
MINUTE
To a solution of 80 mg (0.14 mmol) of the product of Step B dissolved in 1 mL EtOH was added 9 mg (0.20 mmol) of sodium borohydride. The reaction mixture was stirred at RT for 5 min then partitioned between EtOAc and water. The organic layer was separated, dried (MgSO4), filtered and evaporated. The residue was then re...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Ether
Aromatic alcohol
c1cnc2c(c1)CCO2
c1cnc2occc2c1
c1ccccc1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HO-
CCO
null
0.083333
COC(=O)C1(c2ccc(F)c(F)c2)Oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc2C1=O>CCO>Oc1c(-c2ccc(F)c(F)c2)oc2nc(-c3ccc(Cl)cc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2374f352d7f2478f8a9850727af6b546
CN(C)C=O.O=C(Cc1ccc(Cl)cc1)c1ccccc1Cl>>CN(C)C=C(C(=O)c1ccccc1Cl)c1ccc(Cl)cc1
ClC1=C(C=CC=C1)C(CC1=CC=C(C=C1)Cl)=O.CN(C)C=O>>ClC1=C(C=CC=C1)C(C(=CN(C)C)C1=CC=C(C=C1)Cl)=O
O=[CH:4][N:2]([CH3:1])[CH3:3].[CH2:5]([C:6](=[O:7])[c:8]1[cH:9][cH:10][cH:11][cH:12][c:13]1[Cl:14])[c:15]1[cH:16][cH:17][c:18]([Cl:19])[cH:20][cH:21]1>>[CH3:1][N:2]([CH3:3])[CH:4]=[C:5]([C:6](=[O:7])[c:8]1[cH:9][cH:10][cH:11][cH:12][c:13]1[Cl:14])[c:15]1[cH:16][cH:17][c:18]([Cl:19])[cH:20][cH:21]1
CN(C)C=O.O=C(Cc1ccc(Cl)cc1)c1ccccc1Cl
CN(C)C=C(C(=O)c1ccccc1Cl)c1ccc(Cl)cc1
null
null
null
C-C Coupling
Aldol condensation
0834f5811c64eb07624bb510b1953a99dc97db16ae8dba7bd11fc9475950992e
c44260df9c9577267c7fe93dac0096ae481ad05229440bab62074d975d8d7748
[CH]=C(C(=O)c1ccccc1)c1ccccc1
O=[CH;D2;+0:1]-[#7:2](-[C;D1;H3:3])-[C;D1;H3:4].[O;D1;H0:5]=[C:6](-[c:7])-[CH2;D2;+0:8]-[c:9](:[c:10]):[c:11]>>[C;D1;H3:3]-[#7:2](-[C;D1;H3:4])-[CH;D2;+0:1]=[C;H0;D3;+0:8](-[C:6](=[O;D1;H0:5])-[c:7])-[c:9](:[c:10]):[c:11]
null
[]
75
CELSIUS
16
HOUR
To 13.2 g of 1-(2-chlorophenyl)-2-(4-chlorophenyl)ethanone in 100 mL of DMF was added 23.8 g of N,N-dimethylormamide dimethyl acetal. The mixture was stirred at 75° C. for 16 hours. The solution was then concentrated and used without further purification in the next step. Conditions: See reaction.notes.procedure_detail...
10.6084/m9.figshare.5104873.v1
null
Ketone.Tertiary amide
Enamine
null
null
c1ccccc1.c1ccccc1
HO-
null
75
16
CN(C)C=O.O=C(Cc1ccc(Cl)cc1)c1ccccc1Cl>>CN(C)C=C(C(=O)c1ccccc1Cl)c1ccc(Cl)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a4bf6cda5e1b41fbb814ac2110f72af8
CN(C)C=C(C(=O)c1ccccc1Cl)c1ccc(Cl)cc1.N#CCC(N)=O>>N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
ClC1=C(C=CC=C1)C(C(=CN(C)C)C1=CC=C(C=C1)Cl)=O.C(#N)CC(=O)N.[H-].[Na+]>>ClC1=C(C=CC=C1)C1=C(C=C(C(N1)=O)C#N)C1=CC=C(C=C1)Cl
CN(C)[CH:4]=[C:5]([c:6]1[cH:7][cH:8][c:9]([Cl:10])[cH:11][cH:12]1)[C:13](=O)[c:14]1[cH:15][cH:16][cH:17][cH:18][c:19]1[Cl:20].[N:1]#[C:2][CH2:3][C:22]([NH2:21])=[O:23]>>[N:1]#[C:2][c:3]1[cH:4][c:5](-[c:6]2[cH:7][cH:8][c:9]([Cl:10])[cH:11][cH:12]2)[c:13](-[c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]2[Cl:20])[nH:21][c:22]1=...
CN(C)C=C(C(=O)c1ccccc1Cl)c1ccc(Cl)cc1.N#CCC(N)=O
N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
null
null
CN(C)C=O
Aromatic Heterocycle Formation
OtherReaction
60e6cdceb0baa245fe4412e5afd8e8b3b5ab470991e8279dcbe754fb697cedb2
9bf1fd3c6bd3248cd0029464a9f1478a19f5ad042fa396153933395993aab801
O=c1ccc(-c2ccccc2)c(-c2ccccc2)[nH]1
C-N(-C)-[CH;D2;+0:1]=[C;H0;D3;+0:2](-[C;H0;D3;+0:3](=O)-[c;H0;D3;+0:4](:[c:5]:[c:6]):[c:7](-[Cl;D1;H0:8]):[c:9])-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14].[N;D1;H0:15]#[C:16]-[CH2;D2;+0:17]-[C;H0;D3;+0:18](-[NH2;D1;+0:19])=[O;D1;H0:20]>>[Cl;D1;H0:8]-[c:7](:[c:9]):[c;H0;D3;+0:4](-[c;H0;D3;+0:3]1:[nH;D2;+0:19]:[c;H0;...
null
[]
95
CELSIUS
null
null
A solution of the crude product from step A dissolved in 80 mL of DMF containing 4.4 mL methanol and 4.61 g cyanoacetamide was transferred by cannula into a flask containing a suspension of NaH (4.98 g, 60% dispersion in mineral oil, freed of excess oil by washing with hexane just prior to use) in DMF (40 mL). The solu...
10.6084/m9.figshare.5104873.v1
null
Enamine.Ketone.Primary amide
null
null
c1cnccc1
c1cnccc1.c1ccccc1.c1ccccc1
HO-
CN(C)C=O
95
null
CN(C)C=C(C(=O)c1ccccc1Cl)c1ccc(Cl)cc1.N#CCC(N)=O>CN(C)C=O>N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1947bd8bee374badb21ae13f23022d0b
CC(C)(C)C(=O)CBr.N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>>CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ClC1=C(C=CC=C1)C1=C(C=C(C(N1)=O)C#N)C1=CC=C(C=C1)Cl.C(=O)([O-])[O-].[Cs+].[Cs+].BrCC(C(C)(C)C)=O>>NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)C(C(C)(C)C)=O
Br[CH2:7][C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])=[O:6].[O:8]=[c:9]1[nH:10][c:11](-[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[Cl:18])[c:19](-[c:20]2[cH:21][cH:22][c:23]([Cl:24])[cH:25][cH:26]2)[cH:27][c:28]1[C:29]#[N:30]>>[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[c:7]1[o:8][c:9]2[n:10][c:11](-[c:12]3[cH:13][cH:14][cH:15...
CC(C)(C)C(=O)CBr.N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
null
null
C(C)(=O)OCC.CN(C)C=O
Aromatic Heterocycle Formation
OtherReaction
1c3dde6f8fb234f99de372746776db1852e1e639963c229bf01260e389d5e88d
481fee288c2b1a3101ebae707e584a0e925bd48483299d9da5a41b1420634672
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
Br-[CH2;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[c:10](-[c:11]):[nH;D2;+0:12]:[c;H0;D3;+0:13]:1=[O;H0;D1;+0:14]>>[C:3]-[C:2](=[O;D1;H0:4])-[c;H0;D3;+0:1]1:[o;H0;D2;+0:14]:[c;H0;D3;+0:13]2:[n;H0;D2;+0:12]:[c:10](-[c:11]):[c:9]:[c:8]:[c:7]:2:[c;H0;D3;+0:6]:1-[NH2;D1;+0:5]
null
[]
null
null
17
HOUR
To a solution of 0.5 g (1.46 mmol) of the product of Step B in 10 mL DMF was added 0.954 g Cs2CO3 and 0.197 mL of 1-bromopinacolone. The reaction was stirred 17 hours at room temperature at which point the reaction mixture was diluted with ethyl acetate and washed with saturated NaCl/NaHCO3 solution (1:1). The residue ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Nitrile
Ketone.Primary amine
c1cnccc1
c1cnc2occc2c1
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HBr
C(C)(=O)OCC.CN(C)C=O
null
17
CC(C)(C)C(=O)CBr.N#Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>C(C)(=O)OCC.CN(C)C=O>CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-55de1cf4dad34fd0a88cd397f786f4e7
CN(CCO)C(=O)C(=O)Nc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12>>CN1CCN(c2c(C(=O)C(C)(C)C)oc3nc(-c4ccccc4Cl)c(-c4ccc(Cl)cc4)cc23)C(=O)C1=O
ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2NC(C(=O)N(C)CCO)=O)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.CC(C)OC(=O)/N=N/C(=O)OC(C)C>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2N2C(C(N(CC2)C)=O)=O)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl
O[CH2:4][CH2:3][N:2]([CH3:1])[C:37]([C:35]([NH:5][c:6]1[c:7]([C:8](=[O:9])[C:10]([CH3:11])([CH3:12])[CH3:13])[o:14][c:15]2[n:16][c:17](-[c:18]3[cH:19][cH:20][cH:21][cH:22][c:23]3[Cl:24])[c:25](-[c:26]3[cH:27][cH:28][c:29]([Cl:30])[cH:31][cH:32]3)[cH:33][c:34]12)=[O:36])=[O:38]>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[c...
CN(CCO)C(=O)C(=O)Nc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
CN1CCN(c2c(C(=O)C(C)(C)C)oc3nc(-c4ccccc4Cl)c(-c4ccc(Cl)cc4)cc23)C(=O)C1=O
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
26d79d8ccb8e97e1e8c40a78dae5e25aa5f79bf63d44c4f52ff9627941de4a23
53e9ea6bdc0d22524e13e79960e55c0106a6cc8b9aed21c29c8c6a7e9792ce5b
O=C1NCCN(c2coc3nc(-c4ccccc4)c(-c4ccccc4)cc23)C1=O
O-[CH2;D2;+0:1]-[C:2]-[#7:3](-[C;D1;H3:4])-[C:5](=[O;D1;H0:6])-[C:7](=[O;D1;H0:8])-[NH;D2;+0:9]-[c:10]1:[c:11]:[c:12](:[#7;a:13]):[#8;a:14]:[c:15]:1-[C:16]=[O;D1;H0:17]>>[#7;a:13]:[c:12]1:[#8;a:14]:[c:15](-[C:16]=[O;D1;H0:17]):[c:10](-[N;H0;D3;+0:9]2-[CH2;D2;+0:1]-[C:2]-[#7:3](-[C;D1;H3:4])-[C:5](=[O;D1;H0:6])-[C:7]-2=...
null
[]
0
CELSIUS
null
null
A 10 mL rb flask was charged with a solution of 0.075 g (0.13 mmol) of the product of Step A and 0.052 g (0.2 mmol) triphenylphosphine in 2 mL THF. The reaction mixture was stirred at 0° C. and 39 μL of diisopropylazodicarboxylate was added dropwise. The reaction mixture was stirred an additional 1 h at room temperatur...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Primary alcohol
Tertiary amide
null
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HO-
C1CCOC1
0
null
CN(CCO)C(=O)C(=O)Nc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12>C1CCOC1>CN1CCN(c2c(C(=O)C(C)(C)C)oc3nc(-c4ccccc4Cl)c(-c4ccc(Cl)cc4)cc23)C(=O)C1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-29f404ef857d4408835b46d31710774a
CO.O=C(O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>>COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
ClC1=C(C=CC=C1)C1=C(C=C(C(N1)=O)C(=O)O)C1=CC=C(C=C1)Cl.S(O)(O)(=O)=O.CO>>ClC1=C(C=CC=C1)C1=C(C=C(C(N1)=O)C(=O)OC)C1=CC=C(C=C1)Cl
[CH3:1][OH:2].O[C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([Cl:12])[cH:13][cH:14]2)[c:15](-[c:16]2[cH:17][cH:18][cH:19][cH:20][c:21]2[Cl:22])[nH:23][c:24]1=[O:25]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([Cl:12])[cH:13][cH:14]2)[c:15](-[c:16]2[cH:17][cH:18][cH:19][cH:20][c:21...
CO.O=C(O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
null
null
null
Protection
Esterification of Carboxylic Acids
9cecdbd189c6f9c3648521d17154d013842a5498de4e76e65efb1d842973340b
af0b8064f2e82ebe66c4c29d2391785ac1b993104265ccdc4d67ca79e36fa3c8
O=c1ccc(-c2ccccc2)c(-c2ccccc2)[nH]1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5](=[O;D1;H0:6]):[#7;a:7]:[c:8].[C;D1;H3:9]-[OH;D1;+0:10]>>[C;D1;H3:9]-[O;H0;D2;+0:10]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5](=[O;D1;H0:6]):[#7;a:7]:[c:8]
null
[]
null
null
null
null
A 250 mL rb flask equipped with a magnetic stir bar was charged with 6.68 g (19.0 mmol) of the product of Step A, 100 mL methanol, 3 mL of concentrated sulfuric acid and the suspension was refluxed overnight. The resulting clear solution was then cooled to room temperature and evaporated. The residue was partitioned be...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Methanol
Ester
null
null
c1cnccc1.c1ccccc1.c1ccccc1
HO-
null
null
null
CO.O=C(O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>>COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7fd2ced16c8e4fd7949b21830373d6d1
CC(C)(C)C(=O)CBr.COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>>COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
ClC1=C(C=CC=C1)C1=C(C=C(C(N1)=O)C(=O)OC)C1=CC=C(C=C1)Cl.C(=O)([O-])[O-].[Cs+].[Cs+].BrCC(C(C)(C)C)=O>>ClC1=C(C=CC=C1)C1=NC(=C(C(=O)OC)C=C1C1=CC=C(C=C1)Cl)OCC(C(C)(C)C)=O
Br[CH2:26][C:27](=[O:28])[C:29]([CH3:30])([CH3:31])[CH3:32].[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([Cl:12])[cH:13][cH:14]2)[c:15](-[c:16]2[cH:17][cH:18][cH:19][cH:20][c:21]2[Cl:22])[nH:23][c:24]1=[O:25]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([Cl:12])[cH:13]...
CC(C)(C)C(=O)CBr.COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
017f1986ac01103f0525dbacad19524e64453382475ee28a007aff29ee613a92
ac82728493611c77c7c1994f790cea214315197e0940bdfcb00528b82f40a945
c1ccc(-c2cccnc2-c2ccccc2)cc1
Br-[CH2;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].[C;D1;H3:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[c:9]1:[c:10]:[c:11]:[c:12](-[c:13]):[nH;D2;+0:14]:[c;H0;D3;+0:15]:1=[O;H0;D1;+0:16]>>[C:3]-[C:2](=[O;D1;H0:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:16]-[c;H0;D3;+0:15]1:[n;H0;D2;+0:14]:[c:12](-[c:13]):[c:11]:[c:10]:[c:9]:1-[C:7](=[O;D1;H0:8])-[#8:6...
null
[]
null
null
1
HOUR
A 25 mL rb flask was charged with 1.111 g (2.97 mmol) of the product of Step B, 1.451 g (4.45 mmol) Cs2CO3, 10 mL DMF and finally 0.5 mL (3.71 mmol) of bromopinacolone. The reaction mixture was stirred at room temperature 1 h then partitioned between EtOAc and water. The organic layer was washed with water, brine, then...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone
Ketone.Ether
c1cnccc1
c1ccncc1
c1ccncc1.c1ccccc1.c1ccccc1
HBr
CN(C)C=O
null
1
CC(C)(C)C(=O)CBr.COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>CN(C)C=O>COC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ea6785e61a9d489682d374698133b827
CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O.CC(C)(C)C(=O)CBr>>CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
C(C)(=O)C=1C(NC(=C(C1)C1=CC=C(C=C1)Cl)C1=C(C=CC=C1)Cl)=O.C([O-])([O-])=O.[Cs+].[Cs+].BrCC(C(C)(C)C)=O>>C(C)(=O)C=1C(=NC(=C(C1)C1=CC=C(C=C1)Cl)C1=C(C=CC=C1)Cl)OCC(C(C)(C)C)=O
[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][cH:9][c:10]([Cl:11])[cH:12][cH:13]2)[c:14](-[c:15]2[cH:16][cH:17][cH:18][cH:19][c:20]2[Cl:21])[nH:22][c:23]1=[O:24].Br[CH2:25][C:26](=[O:27])[C:28]([CH3:29])([CH3:30])[CH3:31]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][cH:9][c:10]([Cl:11])[cH:12][cH:13]2)[c:...
CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O.CC(C)(C)C(=O)CBr
CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
017f1986ac01103f0525dbacad19524e64453382475ee28a007aff29ee613a92
ac82728493611c77c7c1994f790cea214315197e0940bdfcb00528b82f40a945
c1ccc(-c2cccnc2-c2ccccc2)cc1
Br-[CH2;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].[C;D1;H3:5]-[C:6](=[O;D1;H0:7])-[c:8]1:[c:9]:[c:10]:[c:11](-[c:12]):[nH;D2;+0:13]:[c;H0;D3;+0:14]:1=[O;H0;D1;+0:15]>>[C:3]-[C:2](=[O;D1;H0:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:15]-[c;H0;D3;+0:14]1:[n;H0;D2;+0:13]:[c:11](-[c:12]):[c:10]:[c:9]:[c:8]:1-[C:6](-[C;D1;H3:5])=[O;D1;H0:7]
null
[]
null
null
1.5
HOUR
To a 25 mL rb flask equipped with a magnetic stir bar was added 0.309 g(0.86 mmol) of the product of Step A, 0.422 g (1.29 mmol) of cesium carbonate, 3 mL DMF and finally 145 μL of 1-bromopinacolone was added. The reaction mixture was stirred at room temperature for 1.5 h then partitioned between EtOAc and water. The o...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone
Ketone.Ether
c1cnccc1
c1ccncc1
c1ccncc1.c1ccccc1.c1ccccc1
HBr
CN(C)C=O
null
1.5
CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O.CC(C)(C)C(=O)CBr>CN(C)C=O>CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3c143f1741694798b05a671e25e7f738
CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C>>Cc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
C(C)(=O)C=1C(=NC(=C(C1)C1=CC=C(C=C1)Cl)C1=C(C=CC=C1)Cl)OCC(C(C)(C)C)=O.N12CCCCCC2=NCCC1>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2C)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl
O=[C:2]([CH3:1])[c:30]1[c:11]([O:10][CH2:3][C:4](=[O:5])[C:6]([CH3:7])([CH3:8])[CH3:9])[n:12][c:13](-[c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]2[Cl:20])[c:21](-[c:22]2[cH:23][cH:24][c:25]([Cl:26])[cH:27][cH:28]2)[cH:29]1>>[CH3:1][c:2]1[c:3]([C:4](=[O:5])[C:6]([CH3:7])([CH3:8])[CH3:9])[o:10][c:11]2[n:12][c:13](-[c:14]3[c...
CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
Cc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
CN(C)C=O
Aromatic Heterocycle Formation
OtherReaction
6658b0feb74b91a7acd0ca4b28442f33718467434cddc811566102deb8a65181
17fbc58a598d113342a42a036a912fac83e383e9122994bfeebfa959aeec122c
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[c:3](:[c:4]):[c:5](-[O;H0;D2;+0:6]-[CH2;D2;+0:7]-[C:8](-[C:9])=[O;D1;H0:10]):[#7;a:11]:[c:12]>>[C:9]-[C:8](=[O;D1;H0:10])-[c;H0;D3;+0:7]1:[o;H0;D2;+0:6]:[c:5](:[#7;a:11]:[c:12]):[c:3](:[c:4]):[c;H0;D3;+0:1]:1-[C;D1;H3:2]
null
[]
150
CELSIUS
null
null
A mixture of 0.432 g (0.95 mmol) of the product of Step B, 250 A (1.67 mmol) of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) in 2 mL DMF was placed in a 10 mL reaction tube of a CEM Corporation Discover 300 Watt microwave reactor. The reaction vessel was sealed, placed in the microwave reactor and heated at 150° C. for 10 ...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone.Ether
Ketone
c1ccncc1
c1cnc2occc2c1
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HO-
CN(C)C=O
150
null
CC(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C>CN(C)C=O>Cc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5d4a5433cbe84b68be4d18623d3dc161
Cc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12>>CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1C=O
C[N+]1(CCOCC1)[O-].ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2C)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl.BrN1C(CCC1=O)=O.N(=NC(C#N)(C)C)C(C#N)(C)C>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2C=O)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl
[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[c:7]1[o:8][c:9]2[n:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[Cl:18])[c:19](-[c:20]3[cH:21][cH:22][c:23]([Cl:24])[cH:25][cH:26]3)[cH:27][c:28]2[c:29]1[CH3:30]>>[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[c:7]1[o:8][c:9]2[n:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][cH...
Cc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1C=O
null
null
C(Cl)(Cl)(Cl)Cl
Oxidation
OtherReaction
f82793a7e1ee6561b7709c4a971f65b04fd777875bf3438ec6d6e1a0cf7ef2e4
4f1055c03ef3f74f7ecbf5450c9237f5c3ae016780958675e61943dfb81da1e6
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
[#7;a:1]:[c:2]1:[#8;a:3]:[c:4](-[C:5]=[O;D1;H0:6]):[c:7](-[CH3;D1;+0:8]):[c:9]:1>>[#7;a:1]:[c:2]1:[#8;a:3]:[c:4](-[C:5]=[O;D1;H0:6]):[c:7](-[CH;D2;+0:8]=[O;D1;H0:10]):[c:9]:1
null
[]
null
null
null
null
A 10 mL rb flask equipped with a magnetic stir bar was charged with 0.227 g (0.52 mmol) of the product of Example 89, 0.101 g (0.57 mmol) of N-bromosuccinimide, 3 mL CCl4 and ca. 5 mg of 2,2′-azobisisobutyronitrile (AIBN). The reaction mixture was heated to reflux under a nitrogen atmosphere for 2 h then cooled to room...
10.6084/m9.figshare.5104873.v1
null
null
Aldehyde
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
Other
C(Cl)(Cl)(Cl)Cl
null
null
Cc1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12>C(Cl)(Cl)(Cl)Cl>CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8d62e65ff015489fb58702512914ae73
CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1C=O.CO>>COC(=O)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
[C-]#N.[Na+].ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2C=O)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl.CO>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2C(=O)OC)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl
[CH:3](=[O:4])[c:5]1[c:6]([C:7](=[O:8])[C:9]([CH3:10])([CH3:11])[CH3:12])[o:13][c:14]2[n:15][c:16](-[c:17]3[cH:18][cH:19][cH:20][cH:21][c:22]3[Cl:23])[c:24](-[c:25]3[cH:26][cH:27][c:28]([Cl:29])[cH:30][cH:31]3)[cH:32][c:33]12.[CH3:1][OH:2]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([C:7](=[O:8])[C:9]([CH3:10])([CH3:11])[CH3...
CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1C=O.CO
COC(=O)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
null
[O-2].[O-2].[Mn+4]
null
Acylation
Oxidation of alcohol and aldehyde to ester
6c2cf9780d2b06093c0103c8dd3456912317575c5e7e70f8999846e7a24bbf0c
df63d853b69ab8d080a5e6aeacb0edaa9eaa2dd261e6fc3594fda9a1c296389c
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
[#7;a:1]:[c:2]1:[#8;a:3]:[c:4](-[C:5]=[O;D1;H0:6]):[c:7](-[CH;D2;+0:8]=[O;D1;H0:9]):[c:10]:1.[C;D1;H3:11]-[OH;D1;+0:12]>>[#7;a:1]:[c:2]1:[#8;a:3]:[c:4](-[C:5]=[O;D1;H0:6]):[c:7](-[C;H0;D3;+0:8](=[O;D1;H0:9])-[O;H0;D2;+0:12]-[C;D1;H3:11]):[c:10]:1
null
[]
null
null
4
HOUR
A 10 mL rb flask equipped with a magnetic stir bar and a septum was charged with a solution of 50 mg (0.11 mmol) of the product of Example 90, in 2 mL MeOH, 24 mg (0.27 mmol) of manganese dioxide and ca. 5 mg of sodium cyanide was added. The reaction mixture was stirred at room temperature for 4 h, then filtered and ev...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Methanol
Ester
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
null
[O-2].[O-2].[Mn+4]
null
4
CC(C)(C)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1C=O.CO>[O-2].[O-2].[Mn+4]>COC(=O)c1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d45f944e0ce54e2692d6389881056355
CC(C)(C)C(=O)CCl.O=Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>>CC(C)(C)C(=O)c1cc2cc(-c3ccc(Cl)cc3)c(-c3ccccc3Cl)nc2o1
ClCC(C(C)(C)C)=O.ClC1=C(C=CC=C1)C1=C(C=C(C(N1)=O)C=O)C1=CC=C(C=C1)Cl.ClCC(C(C)(C)C)=O.C(=O)([O-])[O-].[Cs+].[Cs+].C(=O)([O-])[O-].[Cs+].[Cs+]>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl
Cl[CH2:7][C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])=[O:6].O=[CH:8][c:9]1[cH:10][c:11](-[c:12]2[cH:13][cH:14][c:15]([Cl:16])[cH:17][cH:18]2)[c:19](-[c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]2[Cl:26])[nH:27][c:28]1=[O:29]>>[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[c:7]1[cH:8][c:9]2[cH:10][c:11](-[c:12]3[cH:13][cH:14][c:15]([...
CC(C)(C)C(=O)CCl.O=Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
CC(C)(C)C(=O)c1cc2cc(-c3ccc(Cl)cc3)c(-c3ccccc3Cl)nc2o1
null
null
CCOCC
Aromatic Heterocycle Formation
OtherReaction
c7d63de9e2b9aa67c866fcc5b7e8367f6d86730e213054f205bfc771c9800fac
c44055920a7c123f4a11c0861cb7271b9b4758af86c4c5d6f1ec7b42da62d18e
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
Cl-[CH2;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].O=[CH;D2;+0:5]-[c:6]1:[c:7]:[c:8]:[c:9](-[c:10]):[nH;D2;+0:11]:[c;H0;D3;+0:12]:1=[O;H0;D1;+0:13]>>[C:3]-[C:2](=[O;D1;H0:4])-[c;H0;D3;+0:1]1:[cH;D2;+0:5]:[c:6]2:[c:7]:[c:8]:[c:9](-[c:10]):[n;H0;D2;+0:11]:[c;H0;D3;+0:12]:2:[o;H0;D2;+0:13]:1
null
[]
60
CELSIUS
2
HOUR
To a solution of 0.38 g of the product of Step A dissolved in 3 mL of DW, was added 0.14 mL (1.07 mmol) of 1-chloropinacolone and 0.65 g of Cs2CO3. After stirring for 2 h, another 0.05 mL (0.38 mmol) of 1-chloropinacolone was added and the stirring was continued for another 1 h. Additional 0.325 g (1 mmol) of Cs2CO3 wa...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aldehyde.Ketone
Ketone
c1cnccc1
c1cnc2occc2c1
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
CCOCC
60
2
CC(C)(C)C(=O)CCl.O=Cc1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>CCOCC>CC(C)(C)C(=O)c1cc2cc(-c3ccc(Cl)cc3)c(-c3ccccc3Cl)nc2o1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d705a74c03e9403c99b2e96def32a4aa
CC(=O)OCC(=O)Cl.CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>>CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)C(C(C)(C)O)=O.C(C)(=O)OCC(=O)Cl>>C(C)(=O)OCC(=O)NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)C(C(C)(C)O)=O
Cl[C:6]([CH2:5][O:4][C:2]([CH3:1])=[O:3])=[O:7].[NH2:8][c:9]1[c:10]([C:11](=[O:12])[C:13]([CH3:14])([CH3:15])[OH:16])[o:17][c:18]2[n:19][c:20](-[c:21]3[cH:22][cH:23][cH:24][cH:25][c:26]3[Cl:27])[c:28](-[c:29]3[cH:30][cH:31][c:32]([Cl:33])[cH:34][cH:35]3)[cH:36][c:37]12>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][C:6](=[O:7])[NH:...
CC(=O)OCC(=O)Cl.CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
C(C)#N.C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#8:4]-[C:5](-[C;D1;H3:6])=[O;D1;H0:7].[#7;a:8]:[c:9]1:[#8;a:10]:[c:11](-[C:12]=[O;D1;H0:13]):[c:14](-[NH2;D1;+0:15]):[c:16]:1>>[#7;a:8]:[c:9]1:[#8;a:10]:[c:11](-[C:12]=[O;D1;H0:13]):[c:14](-[NH;D2;+0:15]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#8:4]-[C:5](-[C;D1;H3:6])=[O;D1;H0:7]):[c...
null
[]
null
null
null
null
To a solution of 4.0 g of the product of Example 100 in 25 mL of acetonitrile was added 7.5 mL acetoxy acetylchloride and the reaction mixture was stirred at room temperature. After 50 min the reaction mixture was diluted with CH2Cl2 and washed two times with aqueous sodium bicarbonate. The organic layer was dried over...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
C(C)#N.C(Cl)Cl
null
null
CC(=O)OCC(=O)Cl.CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>C(C)#N.C(Cl)Cl>CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2587e99f20af4b9a95cc53879079e3af
CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12>>CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CO
C(C)(=O)O.[OH-].[Li+].O.C(C)(=O)OCC(=O)NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)C(C(C)(C)O)=O.CO>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2NC(CO)=O)C(C(C)(C)O)=O)C2=CC=C(C=C2)Cl
CC(=O)[O:34][CH2:33][C:31]([NH:30][c:29]1[c:7]([C:5]([C:2]([CH3:1])([CH3:3])[OH:4])=[O:6])[o:8][c:9]2[n:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][cH:16][c:17]3[Cl:18])[c:19](-[c:20]3[cH:21][cH:22][c:23]([Cl:24])[cH:25][cH:26]3)[cH:27][c:28]21)=[O:32]>>[CH3:1][C:2]([CH3:3])([OH:4])[C:5](=[O:6])[c:7]1[o:8][c:9]2[n:10][c:11...
CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CO
null
null
C1CCOC1
Reduction
Hydrolysis or Hydrogenolysis of Carboxylic Esters or Thioesters
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
C-C(=O)-[O;H0;D2;+0:1]-[C:2]-[C:3](=[O;D1;H0:4])-[#7:5]-[c:6]:[c:7]:[#8;a:8]>>[#8;a:8]:[c:7]:[c:6]-[#7:5]-[C:3](=[O;D1;H0:4])-[C:2]-[OH;D1;+0:1]
null
[]
null
null
null
null
Lithium hydroxide-H2O (0.293 g), the product of Step A (3.78 g), and methanol (8.4 mL) were combined in 245 mL of THF and stirred at room temperature. After 5 min 0.50 mL of acetic acid was added and the solution concentrated. The residue was diluted with ethyl acetate and this solution washed two times with aqueous so...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HO-
C1CCOC1
null
null
CC(=O)OCC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12>C1CCOC1>CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)CO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e1aac933471c4119887b78fda5452eab
CC(=O)OC(C)=O.CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>>CC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)C(C(C)(C)O)=O.C(C)(=O)OC(C)=O>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2NC(C)=O)C(C(C)(C)O)=O)C2=CC=C(C=C2)Cl
CC(=O)O[C:2]([CH3:1])=[O:3].[NH2:4][c:5]1[c:6]([C:7](=[O:8])[C:9]([CH3:10])([CH3:11])[OH:12])[o:13][c:14]2[n:15][c:16](-[c:17]3[cH:18][cH:19][cH:20][cH:21][c:22]3[Cl:23])[c:24](-[c:25]3[cH:26][cH:27][c:28]([Cl:29])[cH:30][cH:31]3)[cH:32][c:33]12>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[c:6]([C:7](=[O:8])[C:9]([CH3:10])([CH3:1...
CC(=O)OC(C)=O.CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
CC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
C(C)(=O)O
Acylation
Aminolysis of esters
87d35e51b477fc9a658a6f307eb56d84c8879182772c9dd3a42ec0d584fd2684
627cbc0550c9f51ad0105d9fcf46677e8c93bed87ee95bfe69292a82550c95b7
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[#7;a:4]:[c:5]1:[#8;a:6]:[c:7](-[C:8]=[O;D1;H0:9]):[c:10](-[NH2;D1;+0:11]):[c:12]:1>>[#7;a:4]:[c:5]1:[#8;a:6]:[c:7](-[C:8]=[O;D1;H0:9]):[c:10](-[NH;D2;+0:11]-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3]):[c:12]:1
null
[]
85
CELSIUS
null
null
The product of Example 100 (0.200 g), acetic anhydride (1.25 mL) and acetic acid (0.25 mL) were combined and then heated to 85° C. After 3 h the reaction was concentrated and the residue was dissolved in dichloromethane and washed twice with aqueous sodium bicarbonate. The solution was then concentrated and the residue...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Primary amine
Secondary amide
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HO-
C(C)(=O)O
85
null
CC(=O)OC(C)=O.CC(C)(O)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N>C(C)(=O)O>CC(=O)Nc1c(C(=O)C(C)(C)O)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c381bed665bb4627a586bfbdff44fdf8
CC(=O)OCC(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12>>O=C(CO)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)C(=O)C=2C=NC=CC2.C(C)(=O)OCC(=O)Cl>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2NC(CO)=O)C(=O)C=2C=NC=CC2)C2=CC=C(C=C2)Cl
CC(=O)[O:4][CH2:3][C:2](Cl)=[O:1].[NH2:5][c:6]1[c:7]([C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][n:14][cH:15]2)[o:16][c:17]2[n:18][c:19](-[c:20]3[cH:21][cH:22][cH:23][cH:24][c:25]3[Cl:26])[c:27](-[c:28]3[cH:29][cH:30][c:31]([Cl:32])[cH:33][cH:34]3)[cH:35][c:36]12>>[O:1]=[C:2]([CH2:3][OH:4])[NH:5][c:6]1[c:7]([C:8](=[O:9])...
CC(=O)OCC(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
O=C(CO)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
null
Acylation
OtherReaction
8239c8557518ad9a51ed2d39c8a2c37cf919e23e81df767084f341a4c55fccb6
85d144b1d3fe1a2e0dfc6c909128903cc17adef9115f74214503f6a8fa9c284a
O=C(c1cccnc1)c1cc2cc(-c3ccccc3)c(-c3ccccc3)nc2o1
C-C(=O)-[O;H0;D2;+0:1]-[C:2]-[C;H0;D3;+0:3](-Cl)=[O;D1;H0:4].[#7;a:5]:[c:6]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:11](-[NH2;D1;+0:12]):[c:13]:1>>[#7;a:5]:[c:6]1:[#8;a:7]:[c:8](-[C:9]=[O;D1;H0:10]):[c:11](-[NH;D2;+0:12]-[C;H0;D3;+0:3](=[O;D1;H0:4])-[C:2]-[OH;D1;+0:1]):[c:13]:1
null
[]
null
null
null
null
Using the general acylating procedure described in Example 18, the product of Example 157 was reacted with acetoxyacetyl chloride and then subjected to the general ester hydrolysis procedure described in Example 25 to afford the title compound. HPLC/MS: 518.0 (M+1), 520.0 (M+3); Rt=3.52 min. Conditions: See reaction.no...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ester.Primary amine
Secondary amide.Primary alcohol
null
null
c1ccncc1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HCl
null
null
null
CC(=O)OCC(=O)Cl.Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12>>O=C(CO)Nc1c(C(=O)c2cccnc2)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8aaed631857a4993a8ca04b643cc93d8
CC(C)(C)S(=O)(=O)COc1nc(-c2ccccc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>>CC(C)(C)S(=O)(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
C(C)(C)(C)S(=O)(=O)COC1=C(C#N)C=C(C(=N1)C1=C(C=CC=C1)Cl)C1=CC=C(C=C1)Cl.C[Si](C)(C)[N-][Si](C)(C)C.[Li+]>>C(C)(C)(C)S(=O)(=O)C1=C(C=2C(=NC(=C(C2)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)O1)N
[CH3:1][C:2]([CH3:3])([CH3:4])[S:5](=[O:6])(=[O:7])[CH2:8][O:9][c:10]1[n:11][c:12](-[c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]2[Cl:19])[c:20](-[c:21]2[cH:22][cH:23][c:24]([Cl:25])[cH:26][cH:27]2)[cH:28][c:29]1[C:30]#[N:31]>>[CH3:1][C:2]([CH3:3])([CH3:4])[S:5](=[O:6])(=[O:7])[c:8]1[o:9][c:10]2[n:11][c:12](-[c:13]3[cH:14]...
CC(C)(C)S(=O)(=O)COc1nc(-c2ccccc2Cl)c(-c2ccc(Cl)cc2)cc1C#N
CC(C)(C)S(=O)(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
null
null
C1CCOC1.CN(C)C=O
Aromatic Heterocycle Formation
OtherReaction
310e82a1a04ad8be5cc811c019c822a32b44ad18376ea0176a8296685624b50f
1840d341887117642bffcff327c44a81dcd63e1f29237a5b99bb06120b967248
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
[C:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[CH2;D2;+0:5]-[O;H0;D2;+0:6]-[c:7](:[#7;a:8]:[c:9]):[c:10](-[C;H0;D2;+0:11]#[N;H0;D1;+0:12]):[c:13]>>[C:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c;H0;D3;+0:5]1:[o;H0;D2;+0:6]:[c:7](:[#7;a:8]:[c:9]):[c:10](:[c:13]):[c;H0;D3;+0:11]:1-[NH2;D1;+0:12]
null
[]
null
null
null
null
To a stirred solution of 1.87 g (3.9 mmol) of the product of Step B in 24 mL of DMF at 0° C. was added 7.9 mL of a 1.0 M solution of lithium bis(trimethylsilyl)amide in THF. The reaction mixture was stirred an addition 5 min then it was quenched with 0.45 mL of acetic acid and then partitioned between ethyl acetate and...
10.6084/m9.figshare.5104873.v1
null
Ether.Nitrile
Primary amine
c1ccncc1
c1cnc2occc2c1
c1cnc2occc2c1.c1ccccc1.c1ccccc1
null
C1CCOC1.CN(C)C=O
null
null
CC(C)(C)S(=O)(=O)COc1nc(-c2ccccc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>C1CCOC1.CN(C)C=O>CC(C)(C)S(=O)(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0072402313da45f9b61c45596ccdd4e7
CCOC(=O)COc1nc(-c2ccccc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>>CCOC(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
C(C)OC(COC1=NC(=C(C=C1C#N)C1=CC=C(C=C1)Cl)C1=C(C=CC=C1)Cl)=O.C[Si](C)(C)[NH-].C[Si](C)(C)[NH-].[Li+].[Li+]>>NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][O:7][c:8]1[n:9][c:10](-[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[Cl:17])[c:18](-[c:19]2[cH:20][cH:21][c:22]([Cl:23])[cH:24][cH:25]2)[cH:26][c:27]1[C:28]#[N:29]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[o:7][c:8]2[n:9][c:10](-[c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[Cl:17])[c:18]...
CCOC(=O)COc1nc(-c2ccccc2Cl)c(-c2ccc(Cl)cc2)cc1C#N
CCOC(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
null
null
C1CCOC1.CN(C)C=O
Aromatic Heterocycle Formation
OtherReaction
59bcb1d0292a9d6aab4c779dc11fad7b9f43062efa223c362ac1ee6a27f4c785
9dcfc7fb45090136d7ea5d1e73f2fc7bd6ce09ea58bac801b2d4160abff5cb53
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH2;D2;+0:5]-[O;H0;D2;+0:6]-[c:7](:[#7;a:8]:[c:9]):[c:10](-[C;H0;D2;+0:11]#[N;H0;D1;+0:12]):[c:13]>>[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[c;H0;D3;+0:5]1:[o;H0;D2;+0:6]:[c:7](:[#7;a:8]:[c:9]):[c:10](:[c:13]):[c;H0;D3;+0:11]:1-[NH2;D1;+0:12]
null
[]
null
null
20
MINUTE
To a magnetically stirred solution of 2.69 g (6.30 mmol) of the product of Step A dissolved in 60 mL of DMF was slowly added 12.6 mL of a 1 M solution of lithium bis(trimethylsilylamide) in THF at 0° C. The reaction mixture was stirred at room temperature for 20 min then partitioned between EtOAc and 10% aq. NaHSO4. Th...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether.Nitrile
Ester.Primary amine
c1ccncc1
c1cnc2occc2c1
c1cnc2occc2c1.c1ccccc1.c1ccccc1
null
C1CCOC1.CN(C)C=O
null
0.333333
CCOC(=O)COc1nc(-c2ccccc2Cl)c(-c2ccc(Cl)cc2)cc1C#N>C1CCOC1.CN(C)C=O>CCOC(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4e819361b5db4ebbb47b90be7f1b7076
CCN(CC)CC.CCOC(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F>>CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F
ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2NC(C(F)(F)F)=O)C(=O)OCC)C2=CC=C(C=C2)Cl.C(C)N(CC)CC.C[Al](C)C>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2NC(C(F)(F)F)=O)C(=O)N(CC)CC)C2=CC=C(C=C2)Cl
CC[N:3]([CH2:2][CH3:1])[CH2:4][CH3:5].CCO[C:6](=[O:7])[c:8]1[o:9][c:10]2[n:11][c:12](-[c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[Cl:19])[c:20](-[c:21]3[cH:22][cH:23][c:24]([Cl:25])[cH:26][cH:27]3)[cH:28][c:29]2[c:30]1[NH:31][C:32](=[O:33])[C:34]([F:35])([F:36])[F:37]>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[C:6](=[O:7])[c:...
CCN(CC)CC.CCOC(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F
CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F
null
null
C(Cl)Cl.C1(=CC=CC=C1)C
Acylation
OtherReaction
5b22e18c1bbe6b29953993bf715f188ab0e7b9200aa9e656c76da73ed45c630e
13232343996a06c885abe6305a0393a1c1a027e6b07bf37e1b7c416b421816a0
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#8;a:5]:[c:6]:[#7;a:7].C-C-[N;H0;D3;+0:8](-[C:9]-[C;D1;H3:10])-[C:11]-[C;D1;H3:12]>>[#7;a:7]:[c:6]:[#8;a:5]:[c:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:8](-[C:9]-[C;D1;H3:10])-[C:11]-[C;D1;H3:12]):[c:4]
null
[]
null
null
30
MINUTE
To a magnetically stirred solution of 0.119 mL (1.15 mmol) of triethylamine in 5 mL toluene was added 0.575 mL (1.15 mmol) of a 2.0 M solution of trimethylaluminum in toluene at 0° C. The reaction mixture was allowed to warm to room temperature and was stirred for 30 min. A solution of 0.300 g (0.57 mmol) of the produc...
10.6084/m9.figshare.5104873.v1
null
Ester.Tertiary amine
Tertiary amide
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
HO-
C(Cl)Cl.C1(=CC=CC=C1)C
null
0.5
CCN(CC)CC.CCOC(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F>C(Cl)Cl.C1(=CC=CC=C1)C>CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7ac6da8dab584ebf9629637fb9e6f584
CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F>>CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2NC(C(F)(F)F)=O)C(=O)N(CC)CC)C2=CC=C(C=C2)Cl.C([O-])([O-])=O.[K+].[K+].O>>NC1=C(OC2=NC(=C(C=C21)C2=CC=C(C=C2)Cl)C2=C(C=CC=C2)Cl)C(=O)N(CC)CC
O=C(C(F)(F)F)[NH:31][c:30]1[c:8]([C:6]([N:3]([CH2:2][CH3:1])[CH2:4][CH3:5])=[O:7])[o:9][c:10]2[n:11][c:12](-[c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[Cl:19])[c:20](-[c:21]3[cH:22][cH:23][c:24]([Cl:25])[cH:26][cH:27]3)[cH:28][c:29]21>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[C:6](=[O:7])[c:8]1[o:9][c:10]2[n:11][c:12](-[c:13...
CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F
CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
null
null
CO
Reduction
Hydrogenolysis of amides/imides/carbamates
44b36597c7daf0608965c52c8db8a9220c21d9447ce54e0af375898475f3493f
caaeb83af2cb178156ae90fe7f610a106cd4bb5397d23f56d37a7fe11e2668ed
c1ccc(-c2cc3ccoc3nc2-c2ccccc2)cc1
F-C(-F)(-F)-C(=O)-[NH;D2;+0:1]-[c:2]1:[c:3]:[c:4](:[#7;a:5]):[#8;a:6]:[c:7]:1-[C:8](-[#7:9])=[O;D1;H0:10]>>[#7:9]-[C:8](=[O;D1;H0:10])-[c:7]1:[#8;a:6]:[c:4](:[#7;a:5]):[c:3]:[c:2]:1-[NH2;D1;+0:1]
null
[]
60
CELSIUS
3
HOUR
To a magnetically stirred solution of 0.273 g (0.50 mmol) of the product of Example 182 in 5 mL MeOH was added 0.343 g (0.248 mmol) of potassium carbonate and 0.5 mL water. The reaction mixture was stirred at 60° C. for 3 h then cooled to room temperature and partitioned between EtOAc and 10% aq. NaHSO4. The organic ex...
10.6084/m9.figshare.5104873.v1
null
Trifluoro group.Secondary amide
Primary amine
null
null
c1cnc2occc2c1.c1ccccc1.c1ccccc1
Other
CO
60
3
CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1NC(=O)C(F)(F)F>CO>CCN(CC)C(=O)c1oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc2c1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a7fe96d87c28497989d234d770dec179
CC(C)(C)C(=O)CBr.Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>>Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
ClC1=C(C=CC=C1)C1=C(C=C(C(N1)=O)C(=O)C=1N(C=CN1)C)C1=CC=C(C=C1)Cl.BrCC(C(C)(C)C)=O.C(=O)([O-])[O-].[Cs+].[Cs+]>>ClC1=C(C=CC=C1)C1=C(C=C(C(=N1)OCC(C(C)(C)C)=O)C(=O)C=1N(C=CN1)C)C1=CC=C(C=C1)Cl
Br[CH2:30][C:31](=[O:32])[C:33]([CH3:34])([CH3:35])[CH3:36].[CH3:1][n:2]1[cH:3][cH:4][n:5][c:6]1[C:7](=[O:8])[c:9]1[cH:10][c:11](-[c:12]2[cH:13][cH:14][c:15]([Cl:16])[cH:17][cH:18]2)[c:19](-[c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]2[Cl:26])[nH:27][c:28]1=[O:29]>>[CH3:1][n:2]1[cH:3][cH:4][n:5][c:6]1[C:7](=[O:8])[c:9]1[c...
CC(C)(C)C(=O)CBr.Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O
Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
017f1986ac01103f0525dbacad19524e64453382475ee28a007aff29ee613a92
ac82728493611c77c7c1994f790cea214315197e0940bdfcb00528b82f40a945
O=C(c1cnc(-c2ccccc2)c(-c2ccccc2)c1)c1ncc[nH]1
Br-[CH2;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].[#7;a:5]:[c:6](-[C:7](=[O;D1;H0:8])-[c:9]1:[c:10]:[c:11]:[c:12](-[c:13]):[nH;D2;+0:14]:[c;H0;D3;+0:15]:1=[O;H0;D1;+0:16]):[#7;a:17]>>[#7;a:5]:[c:6](-[C:7](=[O;D1;H0:8])-[c:9]1:[c:10]:[c:11]:[c:12](-[c:13]):[n;H0;D2;+0:14]:[c;H0;D3;+0:15]:1-[O;H0;D2;+0:16]-[CH2;D2;+0:1]-[C:2](-...
null
[]
null
null
1
HOUR
To a solution of the product of Step A in 4 mL DMF was added 0.125 g (0.698 mmol) of 1-bromopinacolone and 0.455 g (1.39 mmol) of Cs2CO3. The reaction mixture was stirred at room temperature for 1 h, then partitioned between EtOAc and saturated aqueous NaHCO3 solution. The organic layer was separated, washed with aq. N...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone
Ketone.Ether
c1cnccc1
c1ccncc1
c1ncc[nH]1.c1ccncc1.c1ccccc1.c1ccccc1
HBr
CN(C)C=O
null
1
CC(C)(C)C(=O)CBr.Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)[nH]c1=O>CN(C)C=O>Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ba1760b26e374dbd82c6ff5fe2302808
Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C>>Cn1ccnc1-c1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
ClC1=C(C=CC=C1)C1=C(C=C(C(=N1)OCC(C(C)(C)C)=O)C(=O)C=1N(C=CN1)C)C1=CC=C(C=C1)Cl.N12CCCCCC2=NCCC1>>ClC1=C(C=CC=C1)C1=C(C=C2C(=N1)OC(=C2C=2N(C=CN2)C)C(C(C)(C)C)=O)C2=CC=C(C=C2)Cl
O=[C:7]([c:6]1[n:2]([CH3:1])[cH:3][cH:4][n:5]1)[c:35]1[c:16]([O:15][CH2:8][C:9](=[O:10])[C:11]([CH3:12])([CH3:13])[CH3:14])[n:17][c:18](-[c:19]2[cH:20][cH:21][cH:22][cH:23][c:24]2[Cl:25])[c:26](-[c:27]2[cH:28][cH:29][c:30]([Cl:31])[cH:32][cH:33]2)[cH:34]1>>[CH3:1][n:2]1[cH:3][cH:4][n:5][c:6]1-[c:7]1[c:8]([C:9](=[O:10])...
Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C
Cn1ccnc1-c1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
null
null
CN(C)C=O
Aromatic Heterocycle Formation
OtherReaction
6658b0feb74b91a7acd0ca4b28442f33718467434cddc811566102deb8a65181
17fbc58a598d113342a42a036a912fac83e383e9122994bfeebfa959aeec122c
c1ccc(-c2cc3c(-c4ncc[nH]4)coc3nc2-c2ccccc2)cc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4](-[O;H0;D2;+0:5]-[CH2;D2;+0:6]-[C:7](-[C:8])=[O;D1;H0:9]):[#7;a:10]:[c:11])-[c;H0;D3;+0:12]1:[#7;a:13]:[c:14]:[c:15]:[#7;a:16]:1-[C;D1;H3:17]>>[C:8]-[C:7](=[O;D1;H0:9])-[c;H0;D3;+0:6]1:[o;H0;D2;+0:5]:[c:4](:[#7;a:10]:[c:11]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[c;H0;D3;+0:12]1:[#7;a:13]:...
null
[]
150
CELSIUS
null
null
A mixture of 0.094 g (0.18 mmol) of the product of Step B and 0.027 g (0.18 mmol) of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) in 2 mL DMF was placed in a 10 mL reaction tube of a CEM Corporation Discover 300 Watt microwave reactor. The reaction vessel was sealed, placed in the microwave reactor and heated at 150° C. fo...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone.Ether
Ketone
c1ccncc1
c1cnc2occc2c1
c1ncc[nH]1.c1cnc2occc2c1.c1ccccc1.c1ccccc1
HO-
CN(C)C=O
150
null
Cn1ccnc1C(=O)c1cc(-c2ccc(Cl)cc2)c(-c2ccccc2Cl)nc1OCC(=O)C(C)(C)C>CN(C)C=O>Cn1ccnc1-c1c(C(=O)C(C)(C)C)oc2nc(-c3ccccc3Cl)c(-c3ccc(Cl)cc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bf1a1dda016e411284aba31e2971cca8
O=C(CCl)CCl.O=C(N[C@@H](Cc1ccccc1)C(=O)O)OCc1ccccc1>>O=C(N[C@@H](Cc1ccccc1)[C@H](O)CCl)OCc1ccccc1
ClCC(=O)CCl.C(C1=CC=CC=C1)OC(=O)N[C@@H](CC1=CC=CC=C1)C(=O)O.[BH4-].[Na+]>>C(C1=CC=CC=C1)OC(=O)N[C@H]([C@@H](CCl)O)CC1=CC=CC=C1
O=C(CCl)[CH2:14][Cl:15].O=[C:12]([C@@H:4]([NH:3][C:2](=[O:1])[O:16][CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1)[CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1)[OH:13]>>[O:1]=[C:2]([NH:3][C@@H:4]([CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1)[C@H:12]([OH:13])[CH2:14][Cl:15])[O:16][CH2:17][c:18]1[cH:19][cH:20][cH...
O=C(CCl)CCl.O=C(N[C@@H](Cc1ccccc1)C(=O)O)OCc1ccccc1
O=C(N[C@@H](Cc1ccccc1)[C@H](O)CCl)OCc1ccccc1
null
null
CO.O1CCCC1
C-C Coupling
OtherReaction
be975736ea4dc284d6befa072d9777b891132a86c932e209ec3849b788893253
1c7c048f8a75ee2977c3642525e5bc0c5f72d9781847729e637668c64f734260
O=C(NCCc1ccccc1)OCc1ccccc1
Cl-C-C(=O)-[CH2;D2;+0:1]-[Cl;D1;H0:2].O=[C;H0;D3;+0:3](-[O;D1;H1:4])-[C:5](-[C:6])-[#7:7]-[C:8]=[O;D1;H0:9]>>[C:6]-[C:5](-[#7:7]-[C:8]=[O;D1;H0:9])-[C@H;D3;+0:3](-[O;D1;H1:4])-[CH2;D2;+0:1]-[Cl;D1;H0:2]
48.4
[{"value": 43.0, "product": "C(C1=CC=CC=C1)OC(=O)N[C@H]([C@@H](CCl)O)CC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 48.4, "product": "C(C1=CC=CC=C1)OC(=O)N[C@H]([C@@H](CCl)O)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a solution of N-benzyloxycarbonyl-L-phenylalanine chloromethyl ketone (75 g, 0.2 mol) in a mixture of 800 mL of methanol and 800 mL of tetrahydrofuran was added sodium borohydride (13.17 g, 0.348 mol, 1.54 equiv.) over 100 min. The solution was stirred at room temperature for 2 hours and then concentrated in vacuo. ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Carboxylic acid.Ketone
Primary halide.Secondary alcohol
null
null
c1ccccc1.c1ccccc1
HCl
CO.O1CCCC1
null
2
O=C(CCl)CCl.O=C(N[C@@H](Cc1ccccc1)C(=O)O)OCc1ccccc1>CO.O1CCCC1>O=C(N[C@@H](Cc1ccccc1)[C@H](O)CCl)OCc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-628eb046bea2459cafb3dcfec58ecfd5
O=C(N[C@@H](Cc1ccccc1)[C@H](O)CCl)OCc1ccccc1>>O=C(N[C@@H](Cc1ccccc1)[C@H]1CO1)OCc1ccccc1
[OH-].[K+].C(C1=CC=CC=C1)OC(=O)N[C@H]([C@@H](CCl)O)CC1=CC=CC=C1>>C(C1=CC=CC=C1)OC(=O)N[C@H]([C@H]1CO1)CC1=CC=CC=C1
Cl[CH2:13][C@H:12]([C@@H:4]([NH:3][C:2](=[O:1])[O:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1)[OH:14]>>[O:1]=[C:2]([NH:3][C@@H:4]([CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1)[C@H:12]1[CH2:13][O:14]1)[O:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1
O=C(N[C@@H](Cc1ccccc1)[C@H](O)CCl)OCc1ccccc1
O=C(N[C@@H](Cc1ccccc1)[C@H]1CO1)OCc1ccccc1
null
null
ClCCl.C(C)O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis (intra to epoxy)
ebf120e9288f48b61f87dafb00b4bacd480e273fa54208a20ed1d8b8a8581b3e
9d3e82e8fa4f4bc62c1019e0bd869bdb0cf4748977f3c0b945b8ffdfc70126be
O=C(N[C@@H](Cc1ccccc1)[C@H]1CO1)OCc1ccccc1
Cl-[CH2;D2;+0:1]-[C:2](-[C:3])-[OH;D1;+0:4]>>[C:3]-[C:2]1-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-1
77.3
[{"value": 77.0, "product": "C(C1=CC=CC=C1)OC(=O)N[C@H]([C@H]1CO1)CC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.3, "product": "C(C1=CC=CC=C1)OC(=O)N[C@H]([C@H]1CO1)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
A solution of potassium hydroxide (6.52 g. 0.116 mol, 1.2 equiv.) in 970 mL of absolute ethanol was treated with N-benzyloxycarbonyl-3(S)-amino-1-chloro-4-phenyl-2(S)-butanol (32.3 g, 0.097 mol). This solution was stirred at room temperature for 15 minutes and then concentrated in vacuo to give a white solid. The solid...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary alcohol
Ether
null
C1CO1
c1ccccc1.C1CO1.c1ccccc1
HCl
ClCCl.C(C)O
null
0.25
O=C(N[C@@H](Cc1ccccc1)[C@H](O)CCl)OCc1ccccc1>ClCCl.C(C)O>O=C(N[C@@H](Cc1ccccc1)[C@H]1CO1)OCc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-de60f6eb45574755aa855b738efb7294
CN1CCNCC1.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1>>C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)OCc1ccccc1
CN1CCNCC1.CCN(CC)CC.ClS(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C>>CN1CCN(CC1)S(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C
[NH:7]1[CH2:8][CH2:9][N:10]([CH3:11])[CH2:12][CH2:13]1.Cl[S:4]([CH2:3][C@H:2]([CH3:1])[C:14](=[O:15])[O:16][CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1)(=[O:5])=[O:6]>>[CH3:1][C@@H:2]([CH2:3][S:4](=[O:5])(=[O:6])[N:7]1[CH2:8][CH2:9][N:10]([CH3:11])[CH2:12][CH2:13]1)[C:14](=[O:15])[O:16][CH2:17][c:18]1[cH:19][cH:...
CN1CCNCC1.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1
C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)OCc1ccccc1
null
null
C(Cl)Cl
Acylation
Sulfonamide synthesis (Schotten-Baumann) secondary amine
8c5bae95a7afc59a07547e375f0b07a72ef45ce3f019f7996b69ec8802313118
b7aca5a5d690b0846685a854bc946849e1041bfc3965161290b5ffb2821af09e
O=C(CCS(=O)(=O)N1CCNCC1)OCc1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[C:4]-[C:5]-[C:6](-[#8:7])=[O;D1;H0:8].[#7:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[#8:7]-[C:6](=[O;D1;H0:8])-[C:5]-[C:4]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[N;H0;D3;+0:12]1-[C:11]-[C:10]-[#7:9]-[C:14]-[C:13]-1
null
[]
0
CELSIUS
null
null
A 100 mL round bottom flask equipped with magnetic stir bar was charged with 0.42 mL (1.05 eq) N-methyl-piperazine, 1 mL NEt3 and 20 mL CH2Cl2. The solution was cooled to 0° C. and 1.0 g of benzyl 3-chlorosulfonyl-2(R)-methylpropionate from Example 3 in 5 mL CH2Cl2 was added. After 1 hour reaction was concentrated in v...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Sulfonyl halide
Tertiary amine
C1CNCC[NH]1
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1ccccc1
HCl
C(Cl)Cl
0
null
CN1CCNCC1.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1>C(Cl)Cl>C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)OCc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9d7628515bd341bbb48e1be9eb1b5fc1
C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)OCc1ccccc1>>C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)O
CN1CCN(CC1)S(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C>>CN1CCN(CC1)S(=O)(=O)C[C@@H](C(=O)O)C
c1ccc(C[O:16][C:14]([C@@H:2]([CH3:1])[CH2:3][S:4](=[O:5])(=[O:6])[N:7]2[CH2:8][CH2:9][N:10]([CH3:11])[CH2:12][CH2:13]2)=[O:15])cc1>>[CH3:1][C@@H:2]([CH2:3][S:4](=[O:5])(=[O:6])[N:7]1[CH2:8][CH2:9][N:10]([CH3:11])[CH2:12][CH2:13]1)[C:14](=[O:15])[OH:16]
C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)OCc1ccccc1
C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)O
null
[Pd]
CO
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
C1CNCCN1
[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]
null
[]
null
null
null
null
A 100 mL Fisher/Porter vessel was charged with benzyl 3-[(4-methylpiperizin-1-yl)sulfonyl]-2(R)-methylpropionate in 15 mL MeOH with a catalytic amount of 10% Pd—C. Hydrogenation at 50 psi for 48 hours afforded, after filtration through Celite and concentration in vacuo to yield 3-[(4-methylpiperizin-1-yl)sulfonyl]-2(R)...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
C1C[NH]CC[NH]1
Other
[Pd].CO
null
null
C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)OCc1ccccc1>[Pd].CO>C[C@@H](CS(=O)(=O)N1CCN(C)CC1)C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d52e816d05f1498dbac26bd0c69dc46e
C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1.N>>C[C@@H](CS(N)(=O)=O)C(=O)OCc1ccccc1
ClS(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C.N>>NS(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C
Cl[S:4]([CH2:3][C@H:2]([CH3:1])[C:8](=[O:9])[O:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1)(=[O:6])=[O:7].[NH3:5]>>[CH3:1][C@@H:2]([CH2:3][S:4]([NH2:5])(=[O:6])=[O:7])[C:8](=[O:9])[O:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1
C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1.N
C[C@@H](CS(N)(=O)=O)C(=O)OCc1ccccc1
null
null
C(C)(=O)OCC.C(Cl)Cl
Acylation
OtherReaction
672a14b4f1ef0b966898e1b4c118f241f21df1d6e087372155b9d0c840dac61f
29e1633db8f1f00444181a0bcac91d574ed806fddf9165be4c8478fc32a80994
c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[C:4]-[C:5]-[C:6](-[#8:7])=[O;D1;H0:8].[NH3;D0;+0:9]>>[#8:7]-[C:6](=[O;D1;H0:8])-[C:5]-[C:4]-[S;H0;D4;+0:1](-[NH2;D1;+0:9])(=[O;D1;H0:2])=[O;D1;H0:3]
null
[]
-78
CELSIUS
null
null
A 100 mL round bottom flask equipped with magnetic stir bar was charged with 1.22 g of benzyl 3-chlorosulfonyl-2(R)-methylpropionate in 15 mL CH2Cl2 and cooled to −78° C. To this solution was added to 10 mL of liquid ammonia at −78° C. After 20 minutes the reaction was warmed to room temperature, concentrated in vacuo ...
10.6084/m9.figshare.5104873.v1
null
Sulfonyl halide
Sulfonamide
null
null
c1ccccc1
HCl
C(C)(=O)OCC.C(Cl)Cl
-78
null
C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1.N>C(C)(=O)OCC.C(Cl)Cl>C[C@@H](CS(N)(=O)=O)C(=O)OCc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-201cd0be739148328f976d03ae2a2f3d
C[C@@H](CS(N)(=O)=O)C(=O)OCc1ccccc1>>C[C@@H](CS(N)(=O)=O)C(=O)O
NS(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C>>NS(=O)(=O)C[C@@H](C(=O)O)C
c1ccc(C[O:10][C:8]([C@@H:2]([CH3:1])[CH2:3][S:4]([NH2:5])(=[O:6])=[O:7])=[O:9])cc1>>[CH3:1][C@@H:2]([CH2:3][S:4]([NH2:5])(=[O:6])=[O:7])[C:8](=[O:9])[OH:10]
C[C@@H](CS(N)(=O)=O)C(=O)OCc1ccccc1
C[C@@H](CS(N)(=O)=O)C(=O)O
null
[Pd]
CO
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
null
[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]
97.9
[{"value": 97.9, "product": "NS(=O)(=O)C[C@@H](C(=O)O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A 100 mL Fisher/Porter vessel was charged with 1.1 g of crude benzyl 3-aminosulfonyl-2(R)-methylpropionate in 35 mL MeOH and a catalytic amount of 10% Pd—C. The mixture was hydrogenated at 50 psi for 24 hours, filtered through Celite and concentrated in vacuo to yield 700 mg of 3-aminosulfonyl-2(R)-methylpropionic acid...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
null
Other
[Pd].CO
null
24
C[C@@H](CS(N)(=O)=O)C(=O)OCc1ccccc1>[Pd].CO>C[C@@H](CS(N)(=O)=O)C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-32b557efdea34c5b8be247dea7329d6c
CNC.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1>>C[C@@H](CS(=O)(=O)N(C)C)C(=O)OCc1ccccc1
ClS(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C.CNC>>CN(S(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C)C
[NH:7]([CH3:8])[CH3:9].Cl[S:4]([CH2:3][C@H:2]([CH3:1])[C:10](=[O:11])[O:12][CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1)(=[O:5])=[O:6]>>[CH3:1][C@@H:2]([CH2:3][S:4](=[O:5])(=[O:6])[N:7]([CH3:8])[CH3:9])[C:10](=[O:11])[O:12][CH2:13][c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1
CNC.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1
C[C@@H](CS(=O)(=O)N(C)C)C(=O)OCc1ccccc1
null
null
C(Cl)Cl
Acylation
Sulfonamide synthesis (Schotten-Baumann) secondary amine
abeb6d9a0c70fe5baef0a8e555c2cd55ac2317f763ce7a0831775db7a04777d8
b7aca5a5d690b0846685a854bc946849e1041bfc3965161290b5ffb2821af09e
c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[C:4]-[C:5]-[C:6](-[#8:7])=[O;D1;H0:8].[C;D1;H3:9]-[NH;D2;+0:10]-[C;D1;H3:11]>>[#8:7]-[C:6](=[O;D1;H0:8])-[C:5]-[C:4]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[N;H0;D3;+0:10](-[C;D1;H3:9])-[C;D1;H3:11]
null
[]
-78
CELSIUS
null
null
A 100 mL round bottomed flask equipped with magnetic stir bar was charged with 1.7 g benzyl 3-chlorosulfonyl-2(R)-methylpropionate from Example 3 in 25 mL CH2Cl2. The solution was cooled to −78° C. and 15 mL of anhydrous dimethylamine was slowly added. After 30 minutes the reaction was concentrated in vacuo and the res...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Sulfonyl halide
Tertiary amine
null
null
c1ccccc1
HCl
C(Cl)Cl
-78
null
CNC.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1>C(Cl)Cl>C[C@@H](CS(=O)(=O)N(C)C)C(=O)OCc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8439c1cf79f4464094398af5231f416d
C[C@@H](CS(=O)(=O)N(C)C)C(=O)OCc1ccccc1>>C[C@@H](CS(=O)(=O)N(C)C)C(=O)O
CN(S(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C)C>>CN(S(=O)(=O)C[C@@H](C(=O)O)C)C
c1ccc(C[O:12][C:10]([C@@H:2]([CH3:1])[CH2:3][S:4](=[O:5])(=[O:6])[N:7]([CH3:8])[CH3:9])=[O:11])cc1>>[CH3:1][C@@H:2]([CH2:3][S:4](=[O:5])(=[O:6])[N:7]([CH3:8])[CH3:9])[C:10](=[O:11])[OH:12]
C[C@@H](CS(=O)(=O)N(C)C)C(=O)OCc1ccccc1
C[C@@H](CS(=O)(=O)N(C)C)C(=O)O
null
[Pd]
C(C)(=O)O
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
null
[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]
94
[{"value": 94.0, "product": "CN(S(=O)(=O)C[C@@H](C(=O)O)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A 100 mL Fisher/Porter vessel was charged with 1.4 g of benzyl 3-[(dimethylamino)sulfonyl]-2(R)-methylpropionate in 30 mL acetic acid with a catalytic amount of 10% Pd—C. The reaction was hydrogenated at 50 psi for 24 hours, filtered through Celite and concentrated in vacuo. The residue was azeotroped with toluene then...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
null
Other
[Pd].C(C)(=O)O
null
24
C[C@@H](CS(=O)(=O)N(C)C)C(=O)OCc1ccccc1>[Pd].C(C)(=O)O>C[C@@H](CS(=O)(=O)N(C)C)C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ca28cf8a610b4959a5383f714763369d
C1CCNCC1.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1>>C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)OCc1ccccc1
ClS(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C.N1CCCCC1>>N1(CCCCC1)S(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C
[NH:7]1[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1.Cl[S:4]([CH2:3][C@H:2]([CH3:1])[C:13](=[O:14])[O:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)(=[O:5])=[O:6]>>[CH3:1][C@@H:2]([CH2:3][S:4](=[O:5])(=[O:6])[N:7]1[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1)[C:13](=[O:14])[O:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21...
C1CCNCC1.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1
C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)OCc1ccccc1
null
null
C(Cl)Cl
Acylation
Sulfonamide synthesis (Schotten-Baumann) secondary amine
d63e07b47df62aebedb35134f6d0504cfcbed5ccfdec31c2c42bba6875c15fe7
b7aca5a5d690b0846685a854bc946849e1041bfc3965161290b5ffb2821af09e
O=C(CCS(=O)(=O)N1CCCCC1)OCc1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[C:4]-[C:5]-[C:6](-[#8:7])=[O;D1;H0:8].[C:9]-[C:10]-[NH;D2;+0:11]-[C:12]-[C:13]>>[#8:7]-[C:6](=[O;D1;H0:8])-[C:5]-[C:4]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[N;H0;D3;+0:11](-[C:10]-[C:9])-[C:12]-[C:13]
null
[]
0
CELSIUS
1
HOUR
A 100 mL round bottom flask equipped with magnetic stir bar was charged with 1 g benzyl 3-chlorosulfonyl-2(R)-methylpropionate from Example 3 in 25 mL CH2Cl2. The solution was cooled to 0° C. and 4 mL of piperdine was slowly added. The reaction was stirred 1 hour then concentrated in vacuo. The residue was partioned be...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Sulfonyl halide
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccccc1
HCl
C(Cl)Cl
0
1
C1CCNCC1.C[C@@H](CS(=O)(=O)Cl)C(=O)OCc1ccccc1>C(Cl)Cl>C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)OCc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8a2cbf7437764d01a0233567b8192452
C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)OCc1ccccc1>>C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)O
N1(CCCCC1)S(=O)(=O)C[C@@H](C(=O)OCC1=CC=CC=C1)C>>N1(CCCCC1)S(=O)(=O)C[C@@H](C(=O)O)C
c1ccc(C[O:15][C:13]([C@@H:2]([CH3:1])[CH2:3][S:4](=[O:5])(=[O:6])[N:7]2[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)=[O:14])cc1>>[CH3:1][C@@H:2]([CH2:3][S:4](=[O:5])(=[O:6])[N:7]1[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1)[C:13](=[O:14])[OH:15]
C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)OCc1ccccc1
C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)O
null
[Pd]
null
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
C1CCNCC1
[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]
null
[]
null
null
3
HOUR
A 100 mL Fisher/Porter vessel was charged with 1 g of benzyl 3-(1-piperidinyl)sulfonyl-2(R)-methylpropionate 30 mL MeOH and a catalytic amount of 10% Pd—C. The reaction was hydrogenated at 50 psi for 3 hours. After filtration through Celite and concentration in vacuo of 3-(1-piperidinyl)sulfonyl-2(R)-methylpropionic ac...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
C1CC[NH]CC1
Other
[Pd]
null
3
C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)OCc1ccccc1>[Pd]>C[C@@H](CS(=O)(=O)N1CCCCC1)C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-defc4ba15708436b96ff3719a741c0e0
COC(=O)[C@@H](C)CS(=O)(=O)Cl.NC(c1ccccc1)c1ccccc1>>COC(=O)[C@@H](C)CS(=O)(=O)NC(c1ccccc1)c1ccccc1
NC(C1=CC=CC=C1)C1=CC=CC=C1.C(C)N(CC)CC.ClS(=O)(=O)C[C@@H](C(=O)OC)C>>C1(=CC=CC=C1)C(NS(=O)(=O)C[C@@H](C(=O)OC)C)C1=CC=CC=C1
Cl[S:8]([CH2:7][C@@H:5]([C:3]([O:2][CH3:1])=[O:4])[CH3:6])(=[O:9])=[O:10].[NH2:11][CH:12]([c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[c:19]1[cH:20][cH:21][cH:22][cH:23][cH:24]1>>[CH3:1][O:2][C:3](=[O:4])[C@@H:5]([CH3:6])[CH2:7][S:8](=[O:9])(=[O:10])[NH:11][CH:12]([c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[c:19]1[cH:...
COC(=O)[C@@H](C)CS(=O)(=O)Cl.NC(c1ccccc1)c1ccccc1
COC(=O)[C@@H](C)CS(=O)(=O)NC(c1ccccc1)c1ccccc1
null
null
C(Cl)Cl
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
c1ccc(Cc2ccccc2)cc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[C:4]-[C:5]-[C:6](-[#8:7])=[O;D1;H0:8].[NH2;D1;+0:9]-[C:10](-[c:11])-[c:12]>>[#8:7]-[C:6](=[O;D1;H0:8])-[C:5]-[C:4]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[NH;D2;+0:9]-[C:10](-[c:11])-[c:12]
66.4
[{"value": 66.4, "product": "C1(=CC=CC=C1)C(NS(=O)(=O)C[C@@H](C(=O)OC)C)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
A 100 mL round bottom flask equipped with magnetic stir bar was charged with 1 g aminodiphenylmethane, 2 mL triethylamine in 20 mL CH2Cl2. The reaction was cooled to 0° C. and 1 g of methyl 3-chlorosulfonyl-2(R)-methylpropionate was slowly added. The reaction was stirred 1 hour then concentrated in vacuo. The residue w...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccccc1.c1ccccc1
HCl
C(Cl)Cl
0
1
COC(=O)[C@@H](C)CS(=O)(=O)Cl.NC(c1ccccc1)c1ccccc1>C(Cl)Cl>COC(=O)[C@@H](C)CS(=O)(=O)NC(c1ccccc1)c1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4f361e1fb24b4f6abd016d6bd1ac7df4
BrCc1ccccc1.COC(=O)[C@@H](C)CS(=O)(=O)NC(c1ccccc1)c1ccccc1>>COC(=O)[C@@H](C)CS(=O)(=O)N(Cc1ccccc1)C(c1ccccc1)c1ccccc1
C1(=CC=CC=C1)C(NS(=O)(=O)C[C@@H](C(=O)OC)C)C1=CC=CC=C1.C(=O)([O-])[O-].[K+].[K+].C(C1=CC=CC=C1)Br>>C(C1=CC=CC=C1)N(S(=O)(=O)C[C@@H](C(=O)OC)C)C(C1=CC=CC=C1)C1=CC=CC=C1
Br[CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1.[CH3:1][O:2][C:3](=[O:4])[C@@H:5]([CH3:6])[CH2:7][S:8](=[O:9])(=[O:10])[NH:11][CH:19]([c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1)[c:26]1[cH:27][cH:28][cH:29][cH:30][cH:31]1>>[CH3:1][O:2][C:3](=[O:4])[C@@H:5]([CH3:6])[CH2:7][S:8](=[O:9])(=[O:10])[N:11]([CH2:12][c:13...
BrCc1ccccc1.COC(=O)[C@@H](C)CS(=O)(=O)NC(c1ccccc1)c1ccccc1
COC(=O)[C@@H](C)CS(=O)(=O)N(Cc1ccccc1)C(c1ccccc1)c1ccccc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0fe6648877a29ae177a907a0d252f35d8beab440bf428116c5424a67bc0e72cd
0b054affe7e4bb904ceae512aabc19d89c93551cb46dfbc6f220fc85e5eeff75
c1ccc(CNC(c2ccccc2)c2ccccc2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[#16:6](=[O;D1;H0:7])(=[O;D1;H0:8])-[NH;D2;+0:9]-[C:10](-[c:11])-[c:12]>>[C:5]-[#16:6](=[O;D1;H0:7])(=[O;D1;H0:8])-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10](-[c:11])-[c:12]
null
[]
null
null
8
HOUR
A 100 mL round bottom flask equipped with magnetic stir bar and N2 inlet was charged with 1.11 g of methyl 3-[N-(diphenylmethyl) aminosulfonyl]-2(R)-methylpropionate, 447 mg K2CO3, 347 mL benzyl bromide in 20 mL DMF. The reaction was stirred overnight, concentrated in vacuo and partioned between ethyl acetate and water...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Primary halide
Tertiary amine
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HBr
CN(C)C=O
null
8
BrCc1ccccc1.COC(=O)[C@@H](C)CS(=O)(=O)NC(c1ccccc1)c1ccccc1>CN(C)C=O>COC(=O)[C@@H](C)CS(=O)(=O)N(Cc1ccccc1)C(c1ccccc1)c1ccccc1