dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
time_units
large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ae2bce0aa2434bbe9aa4872d5d9cafd6
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2(O)C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
[Si](C)(C)(C(C)(C)C)OCCCC1=CC=C(OCC#CC2(C(COC3=CC(=CC=C23)OCOC)(C)C2=CC=C(C=C2)OCOC)O)C=C1.[Si](C)(C)(C(C)(C)C)OCCCCCCCC#CC1C(CSC2=CC(=CC=C12)OC)(C)C1=CC=C(C=C1)OC>>[Si](C)(C)(C(C)(C)C)OCCCC1=CC=C(OCC#CC2C(COC3=CC(=CC=C23)OCOC)(C)C2=CC=C(C=C2)OCOC)C=C1
O[C:23]1([C:24]#[C:25][CH2:26][O:27][c:28]2[cH:29][cH:30][c:31]([CH2:32][CH2:33][CH2:34][O:35][Si:36]([CH3:37])([CH3:38])[C:39]([CH3:40])([CH3:41])[CH3:42])[cH:43][cH:44]2)[C:9]([c:8]2[cH:7][cH:6][c:5]([O:4][CH2:3][O:2][CH3:1])[cH:46][cH:45]2)([CH3:10])[CH2:11][O:12][c:13]2[cH:14][c:15]([O:16][CH2:17][O:18][CH3:19])[cH...
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2(O)C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
null
null
null
Reduction
OtherReaction
d9ad9de0a2df8f543d454c115f7a58d9a012b1cbcc0f40fa0bf7cc7b376ca1e8
dfa71f841ee148297c95b5d95b7150768ab9356304fca8dbfde20c6dadd639d3
C(#CC1c2ccccc2OCC1c1ccccc1)COc1ccccc1
O-[C;H0;D4;+0:1]1(-[C:2]#[C:3]-[C:4])-[c:5](:[c:6]):[c:7]-[#8:8]-[C:9]-[C:10]-1(-[C;D1;H3:11])-[c:12]>>[C:4]-[C:3]#[C:2]-[CH;D3;+0:1]1-[c:5](:[c:6]):[c:7]-[#8:8]-[C:9]-[C:10]-1(-[C;D1;H3:11])-[c:12]
null
[]
null
null
null
null
The title compound was prepared from 4-{3-[4-(3-t-butyldimethylsilyloxypropyl)phenoxy]-1-propynyl}-7-methoxymethyloxy-3-(4-methoxymethyloxyphenyl)-3-methylchroman-4-ol according to the same method for the synthesis of 4-[9-(t-butyldimethylsilyloxy)-1-nonynyl]-7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman described ...
10.6084/m9.figshare.5104873.v1
null
Tertiary alcohol
null
c1ccc2c(c1)CCCO2
c1ccc2c(c1)CCCO2
c1ccccc1.c1ccc2c(c1)CCCO2.c1ccccc1
Other
null
null
null
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2(O)C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-98c2443a642f46f187349ca6df202f00
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
[Si](C)(C)(C(C)(C)C)OCCCC1=CC=C(OCC#CC2C(COC3=CC(=CC=C23)OCOC)(C)C2=CC=C(C=C2)OCOC)C=C1.[Si](C)(C)(C(C)(C)C)OCCCCCCCCCC1C(CSC2=CC(=CC=C12)OC)(C)C1=CC=C(C=C1)OC>>[Si](C)(C)(C(C)(C)C)OCCCC1=CC=C(OCCCC2C(COC3=CC(=CC=C23)OCOC)(C)C2=CC=C(C=C2)OCOC)C=C1
[CH3:1][O:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8]([C:9]2([CH3:10])[CH2:11][O:12][c:13]3[cH:14][c:15]([O:16][CH2:17][O:18][CH3:19])[cH:20][cH:21][c:22]3[CH:23]2[C:24]#[C:25][CH2:26][O:27][c:28]2[cH:29][cH:30][c:31]([CH2:32][CH2:33][CH2:34][O:35][Si:36]([CH3:37])([CH3:38])[C:39]([CH3:40])([CH3:41])[CH3:42])[cH:43][cH:44]2)...
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
null
null
null
Reduction
OtherReaction
2bb8d5b532a2781e0a7c069a5cd3e8a7e8d44660c0ec1d9e17c04d8ba2cb383b
1990560e9c55934bde8ca0feaed9c61d80f37f94f0cf240a9929dc374d0a33aa
c1ccc(OCCCC2c3ccccc3OCC2c2ccccc2)cc1
[#8:1]-[C:2]-[C;H0;D2;+0:3]#[C;H0;D2;+0:4]-[C:5](-[C:6])-[c:7]>>[#8:1]-[C:2]-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[C:5](-[C:6])-[c:7]
null
[]
null
null
null
null
The title compound was prepared from 4-{3-[4-(3-t-butyldimethylsilyloxypropyl)phenoxy]-1-propynyl}-7-methoxymethyloxy-3-(4-methoxymethyloxyphenyl)-3-methylchroman according to the same method for the synthesis of 4-[9-(t-butyldimethylsilyloxy)-1-nonyl]-7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman described in Inte...
10.6084/m9.figshare.5104873.v1
null
Alkyne
null
null
null
c1ccccc1.c1ccc2c(c1)CCCO2.c1ccccc1
null
null
null
null
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2C#CCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6c73446eef51478ba3bef8d5670c76fa
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO)cc2)cc1
[Si](C)(C)(C(C)(C)C)OCCCC1=CC=C(OCCCC2C(COC3=CC(=CC=C23)OCOC)(C)C2=CC=C(C=C2)OCOC)C=C1.OCCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC>>OCCCC1=CC=C(OCCCC2C(COC3=CC(=CC=C23)OCOC)(C)C2=CC=C(C=C2)OCOC)C=C1
CC(C)(C)[Si](C)(C)[O:35][CH2:34][CH2:33][CH2:32][c:31]1[cH:30][cH:29][c:28]([O:27][CH2:26][CH2:25][CH2:24][CH:23]2[C:9]([c:8]3[cH:7][cH:6][c:5]([O:4][CH2:3][O:2][CH3:1])[cH:39][cH:38]3)([CH3:10])[CH2:11][O:12][c:13]3[cH:14][c:15]([O:16][CH2:17][O:18][CH3:19])[cH:20][cH:21][c:22]32)[cH:37][cH:36]1>>[CH3:1][O:2][CH2:3][O...
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO)cc2)cc1
null
null
null
Deprotection
Alcohol deprotection from silyl ethers
6ff8c9c41093ab5237b871dd4689ba6431022d615e227d3774901a983c846e4b
84d9f5b4e7757c58e584c26c7d52c9a3f594fbcb0c0d22f34765a93a932fcd5b
c1ccc(OCCCC2c3ccccc3OCC2c2ccccc2)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]
null
[]
null
null
null
null
The title compound was prepared from (3RS,4RS)-4-{3-[4-(3-t-butyl-dimethylsilyloxypropyl)phenoxy]-1-propyl}-7-methoxymethyloxy-3-(4-methoxymethyloxyphenyl)-3-methylchroman according to the same method for the synthesis of 4-[9-hydroxy-1-nonyl]-7-methoxymethyloxy-3-(4-methoxymethyloxyphenyl)-3-methylchroman described in...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Primary alcohol
null
null
c1ccccc1.c1ccc2c(c1)CCCO2.c1ccccc1
Other
null
null
null
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO[Si](C)(C)C(C)(C)C)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCOc2ccc(CCCO)cc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cb5613b1b5b74d26bc9c8f8102fa89da
CC(C)(C)OC(=O)CBr.COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(O)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCC(=O)OC(C)(C)C)cc2)cc1
O.C(C)(C)(C)OC(CBr)=O.OC1=CC=C(C=C1)CCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC.[H-].[Na+]>>C(C)(C)(C)OC(=O)COC1=CC=C(C=C1)CCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC
Br[CH2:33][C:34](=[O:35])[O:36][C:37]([CH3:38])([CH3:39])[CH3:40].[CH3:1][O:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8]([C:9]2([CH3:10])[CH2:11][O:12][c:13]3[cH:14][c:15]([O:16][CH2:17][O:18][CH3:19])[cH:20][cH:21][c:22]3[CH:23]2[CH2:24][CH2:25][CH2:26][CH2:27][c:28]2[cH:29][cH:30][c:31]([OH:32])[cH:41][cH:42]2)[cH:43][cH:44...
CC(C)(C)OC(=O)CBr.COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(O)cc2)cc1
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCC(=O)OC(C)(C)C)cc2)cc1
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
50d675b335c583a6ce22e1164b27a78b18b9ca447d45137820c344bcb6369217
0865de4e1853c59ac25437e36fd18b03329566cb9eff4b4f0ce70d5714692fd3
c1ccc(CCCCC2c3ccccc3OCC2c2ccccc2)cc1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5](-[C;D1;H3:6])(-[C;D1;H3:7])-[C;D1;H3:8].[OH;D1;+0:9]-[c:10](:[c:11]):[c:12]>>[C;D1;H3:6]-[C:5](-[C;D1;H3:7])(-[C;D1;H3:8])-[#8:4]-[C:2](=[O;D1;H0:3])-[CH2;D2;+0:1]-[O;H0;D2;+0:9]-[c:10](:[c:11]):[c:12]
99.5
[{"value": 99.5, "product": "C(C)(C)(C)OC(=O)COC1=CC=C(C=C1)CCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
To a solution of 4-[4-(4-hydroxyphenyl)-1-butyl]-7-methoxymethyloxy-3-(4-methoxymethyloxyphenyl)-3-methylchroman (481 mg, 0.976 mmol) in dry tetrahydrofuran (8 ml) was added sodium hydride (22.7 mg, 1.418 mmol) at room temperature and stirred for 20 minutes. Bromoacetic acid tert-butylester (276.7 mg, 1.418 mmol) was a...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Aromatic alcohol
Ester.Ether
null
null
c1ccccc1.c1ccc2c(c1)CCCO2.c1ccccc1
HBr
O1CCCC1
null
0.333333
CC(C)(C)OC(=O)CBr.COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(O)cc2)cc1>O1CCCC1>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCC(=O)OC(C)(C)C)cc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d3ba945d069046049c5a08a5de0469e4
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCC(=O)OC(C)(C)C)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCCO)cc2)cc1
C(C)(=O)OCC.[OH-].[Na+].C(C)(C)(C)OC(=O)COC1=CC=C(C=C1)CCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>OCCOC1=CC=C(C=C1)CCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC
CC(C)(C)O[C:34]([CH2:33][O:32][c:31]1[cH:30][cH:29][c:28]([CH2:27][CH2:26][CH2:25][CH2:24][CH:23]2[C:9]([c:8]3[cH:7][cH:6][c:5]([O:4][CH2:3][O:2][CH3:1])[cH:39][cH:38]3)([CH3:10])[CH2:11][O:12][c:13]3[cH:14][c:15]([O:16][CH2:17][O:18][CH3:19])[cH:20][cH:21][c:22]32)[cH:37][cH:36]1)=[O:35]>>[CH3:1][O:2][CH2:3][O:4][c:5]...
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCC(=O)OC(C)(C)C)cc2)cc1
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCCO)cc2)cc1
null
null
O1CCCC1
Reduction
Reduction of ester to primary alcohol
005ed55ca3498ead0a405ca36187c0e85620a6bf11f425e5d3f35c18fb5c1feb
b685880638f3f6d2edbccd81c5d4aa218aa09f2b7a06a7fe669dee5c38c3c0e3
c1ccc(CCCCC2c3ccccc3OCC2c2ccccc2)cc1
C-C(-C)(-C)-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]-[#8:4]>>[#8:4]-[C:3]-[CH2;D2;+0:1]-[OH;D1;+0:2]
100
[{"value": 100.0, "product": "OCCOC1=CC=C(C=C1)CCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
To a solution of 4-{4-[4-(t-butoxycarbonylmethyloxy)phenyl]-1-butyl}-7-methoxymethyloxy-3-(4-methoxymethyloxyphenyl)-3-methylchroman (744 mg, 1.226 mmol) in dry tetrahydrofuran (10 mi) was added lithium aluminum hydride (71.8 mg, 1.89 mmol) at 0° C. and stirred for 4 h at the room temperature. When the reaction was com...
10.6084/m9.figshare.5104873.v1
null
Ester.Boc
Primary alcohol
null
null
c1ccccc1.c1ccc2c(c1)CCCO2.c1ccccc1
HO-
O1CCCC1
null
4
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCC(=O)OC(C)(C)C)cc2)cc1>O1CCCC1>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCc2ccc(OCCO)cc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f5535ef36f8a41b7b00ca4f5d150d61a
CC(C)(C)[Si](C)(C)OCCCCCCCCCI.COc1ccc2c(c1)OCC(C)(c1cccnc1)C2=O>>COc1ccc2c(c1)OCC(C)(c1cccnc1)C2(O)CCCCCCCCCO[Si](C)(C)C(C)(C)C
[NH4+].[Cl-].COC1=CC=C2C(C(COC2=C1)(C=1C=NC=CC1)C)=O.[Si](C)(C)(C(C)(C)C)OCCCCCCCCCI.[Li]C(C)(C)C>>[Si](C)(C)(C(C)(C)C)OCCCCCCCCCC1(C(COC2=CC(=CC=C12)OC)(C=1C=NC=CC1)C)O
I[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][O:30][Si:31]([CH3:32])([CH3:33])[C:34]([CH3:35])([CH3:36])[CH3:37].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[O:9][CH2:10][C:11]([CH3:12])([c:13]1[cH:14][cH:15][cH:16][n:17][cH:18]1)[C:19]2=[O:20]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7...
CC(C)(C)[Si](C)(C)OCCCCCCCCCI.COc1ccc2c(c1)OCC(C)(c1cccnc1)C2=O
COc1ccc2c(c1)OCC(C)(c1cccnc1)C2(O)CCCCCCCCCO[Si](C)(C)C(C)(C)C
null
null
CCCCC.C(C)OCC.C1CCOC1
C-C Coupling
Grignard_alcohol
3564a312877016c9d06e74226a688b803cc3abe5b2bca6c50de489b2e8dea1a8
afe96a58b8c6ca4e103c0c96e2a417cdee8e581054f8e646150ad555cb751905
c1cncc(C2COc3ccccc3C2)c1
I-[CH2;D2;+0:1]-[C:2]-[C:3].[#7;a:4]:[c:5]:[c:6]-[C:7]1(-[C;D1;H3:8])-[C:9]-[#8:10]-[c:11]:[c:12](:[c:13])-[C;H0;D3;+0:14]-1=[O;H0;D1;+0:15]>>[#7;a:4]:[c:5]:[c:6]-[C:7]1(-[C;D1;H3:8])-[C:9]-[#8:10]-[c:11]:[c:12](:[c:13])-[C;H0;D4;+0:14]-1(-[OH;D1;+0:15])-[CH2;D2;+0:1]-[C:2]-[C:3]
75.1
[{"value": 75.0, "product": "[Si](C)(C)(C(C)(C)C)OCCCCCCCCCC1(C(COC2=CC(=CC=C12)OC)(C=1C=NC=CC1)C)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.1, "product": "[Si](C)(C)(C(C)(C)C)OCCCCCCCCCC1(C(COC2=CC(=CC=C12)OC)(C=1C=NC=CC1)C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
10
MINUTE
To a solution of 9-(t-butyldimethylsilyloxy)nonyl iodide (1.05 g, 2.7 mmol) in pentane (10 ml) and diethylether (7 ml) was added at −78° C. t-BuLi (1.64M in pentane, 3.62 ml, 5.94 mmol), which was stirred for 10 minutes and then stirred for 1 h at room temperature. The mixture was cooled to −78° C. again, and a solutio...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone
Tertiary alcohol
c1ccc2c(c1)CCCO2
c1ccc2c(c1)CCCO2
c1ccc2c(c1)CCCO2.c1ccncc1
I-
CCCCC.C(C)OCC.C1CCOC1
-78
0.166667
CC(C)(C)[Si](C)(C)OCCCCCCCCCI.COc1ccc2c(c1)OCC(C)(c1cccnc1)C2=O>CCCCC.C(C)OCC.C1CCOC1>COc1ccc2c(c1)OCC(C)(c1cccnc1)C2(O)CCCCCCCCCO[Si](C)(C)C(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b681396a40da49328be1769d375a8d89
COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCO)cc1.CS(=O)(=O)Cl>>COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCOS(C)(=O)=O)cc1
O.OCCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)C1=CC=C(C=C1)OCOC.C(C)N(CC)CC.CS(=O)(=O)Cl>>CS(=O)(=O)OCCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)C1=CC=C(C=C1)OCOC
[CH3:1][O:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8]([CH:9]2[CH2:10][O:11][c:12]3[cH:13][c:14]([O:15][CH2:16][O:17][CH3:18])[cH:19][cH:20][c:21]3[CH:22]2[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][OH:32])[cH:37][cH:38]1.Cl[S:33]([CH3:34])(=[O:35])=[O:36]>>[CH3:1][O:2][CH2:3][O:4][c:5]1[cH:6][cH:...
COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCO)cc1.CS(=O)(=O)Cl
COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCOS(C)(=O)=O)cc1
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1ccc(C2COc3ccccc3C2)cc1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6]-[OH;D1;+0:7]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
99
[{"value": 99.0, "product": "CS(=O)(=O)OCCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)C1=CC=C(C=C1)OCOC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.5, "product": "CS(=O)(=O)OCCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)C1=CC=C(C=C1)OCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
45
MINUTE
To a solution of (3RS,4RS)-4-(9-hydroxynonyl)-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)chroman (222 mg, 0.470 mmol) and triethylamine (0.135 ml, 0.961 mmol) in CH2Cl2 (5 ml) at 0° C. under nitrogen was added methanesulfonyl chloride (0.055 ml, 0.71 mmol). The resulting solution was stirred at 0° C. for 45 min, and th...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1ccccc1.c1ccc2c(c1)CCCO2
HCl
C(Cl)Cl
0
0.75
COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCO)cc1.CS(=O)(=O)Cl>C(Cl)Cl>COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCOS(C)(=O)=O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e8908afb197149f1a016045aa0013908
COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1>>Oc1ccc(C2COc3cc(O)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1
O.COCOC1=CC=C2C(C(COC2=C1)C1=CC=C(C=C1)OCOC)CCCCCCCCCSCCCC(C(F)(F)F)(F)F.Cl>>OC1=CC=C2C(C(COC2=C1)C1=CC=C(C=C1)O)CCCCCCCCCSCCCC(C(F)(F)F)(F)F
COC[O:1][c:2]1[cH:3][cH:4][c:5]([CH:6]2[CH2:7][O:8][c:9]3[cH:10][c:11]([O:12]COC)[cH:13][cH:14][c:15]3[CH:16]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][S:26][CH2:27][CH2:28][CH2:29][C:30]([F:31])([F:32])[C:33]([F:34])([F:35])[F:36])[cH:37][cH:38]1>>[OH:1][c:2]1[cH:3][cH:4][c:5]([CH:6]2[CH...
COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1
Oc1ccc(C2COc3cc(O)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1
null
null
CCO
Reduction
OtherReaction
ca434a15af04bd105d14de328e5decdefa40fa872c8bf2d8a06e38dd9d786610
9290d799ef03b273f5a33508bad8fca1206e009b9df18f946351c38e7647a04c
c1ccc(C2COc3ccccc3C2)cc1
C-O-C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].C-O-C-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]
80
[{"value": 80.0, "product": "OC1=CC=C2C(C(COC2=C1)C1=CC=C(C=C1)O)CCCCCCCCCSCCCC(C(F)(F)F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.5, "product": "OC1=CC=C2C(C(COC2=C1)C1=CC=C(C=C1)O)CCCCCCCCCSCCCC(C(F)(F)F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
17
HOUR
To a solution of (3RS,4RS)-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-4-[9-(4,4,5,5,5-pentafluoropentylthio)nonyl]chroman (204 mg, 0.314 mmol) in EtOH (2 ml) was added 6N HCl (0.2 ml, 1.2 mmol). The resulting solution was stirred between 40 and 45° C. for 17 hr, and then poured into H2O. The mixture was extracted with...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Ether
Aromatic alcohol.Aromatic alcohol
null
null
c1ccccc1.c1ccc2c(c1)CCCO2
HO-
CCO
null
17
COCOc1ccc(C2COc3cc(OCOC)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1>CCO>Oc1ccc(C2COc3cc(O)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f9fd6cf2533f4847b46d5d3daee6cddd
Oc1ccc(C2COc3cc(O)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1>>O=S(CCCCCCCCCC1c2ccc(O)cc2OCC1c1ccc(O)cc1)CCCC(F)(F)C(F)(F)F
OC1=CC=C2C(C(COC2=C1)C1=CC=C(C=C1)O)CCCCCCCCCSCCCC(C(F)(F)F)(F)F.O.OOS(=O)[O-].[K+].O>>OC1=CC=C2C(C(COC2=C1)C1=CC=C(C=C1)O)CCCCCCCCCS(=O)CCCC(C(F)(F)F)(F)F
[S:2]([CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH:12]1[c:13]2[cH:14][cH:15][c:16]([OH:17])[cH:18][c:19]2[O:20][CH2:21][CH:22]1[c:23]1[cH:24][cH:25][c:26]([OH:27])[cH:28][cH:29]1)[CH2:30][CH2:31][CH2:32][C:33]([F:34])([F:35])[C:36]([F:37])([F:38])[F:39]>>[O:1]=[S:2]([CH2:3][CH2:4][CH2:5][CH2:6][...
Oc1ccc(C2COc3cc(O)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1
O=S(CCCCCCCCCC1c2ccc(O)cc2OCC1c1ccc(O)cc1)CCCC(F)(F)C(F)(F)F
null
null
C1CCOC1
Oxidation
Sulfanyl to sulfinyl
9edfaf6d72a81452ea8e3a1cdcb10a58409fff36608e97019e7273998b3d5373
f5f6bb6ca76a2267cd589767b4d67e7a17ab1ac383eeb6143dcd5d92e00e1b6a
c1ccc(C2COc3ccccc3C2)cc1
[C:1]-[C:2]-[S;H0;D2;+0:3]-[C:4]-[C:5]>>[C:1]-[C:2]-[S;H0;D3;+0:3](=[O;D1;H0:6])-[C:4]-[C:5]
73
[{"value": 73.0, "product": "OC1=CC=C2C(C(COC2=C1)C1=CC=C(C=C1)O)CCCCCCCCCS(=O)CCCC(C(F)(F)F)(F)F", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
3.5
HOUR
To a solution of (3RS,4RS)-7-hydroxy-3-(4-hydroxyphenyl)-4-[9-(4,4,5,5,5-pentafluoropentylthio)nonyl]chroman (140 mg, 0.250 mmol) and H2O (0.05 ml) in THF (1.2 ml) at 0° C. was added Oxone® (monopersulfate compound; DuPont product) (77 mg, 0.125 mmol). The resulting solution was stirred at 0° C. for 3.5 hr, and then po...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfoxide
null
null
c1ccc2c(c1)CCCO2.c1ccccc1
null
C1CCOC1
0
3.5
Oc1ccc(C2COc3cc(O)ccc3C2CCCCCCCCCSCCCC(F)(F)C(F)(F)F)cc1>C1CCOC1>O=S(CCCCCCCCCC1c2ccc(O)cc2OCC1c1ccc(O)cc1)CCCC(F)(F)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3a47379b3ceb4d8bb2427f79f266f219
C=CCCCCCC(=O)CC(=O)OCC.FC(F)(F)C(F)(F)CCCI>>C=CCCCCCC(=O)C(CCCC(F)(F)C(F)(F)F)C(=O)OCC
O.FC(CCCI)(C(F)(F)F)F.C(C)OC(CC(CCCCCC=C)=O)=O.CC(C)([O-])C.[K+]>>C(C)OC(C(C(CCCCCC=C)=O)CCCC(C(F)(F)F)(F)F)=O
[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8](=[O:9])[CH2:10][C:21](=[O:22])[O:23][CH2:24][CH3:25].I[CH2:11][CH2:12][CH2:13][C:14]([F:15])([F:16])[C:17]([F:18])([F:19])[F:20]>>[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8](=[O:9])[CH:10]([CH2:11][CH2:12][CH2:13][C:14]([F:15])([F:16])[C:17]([F:18])([F:1...
C=CCCCCCC(=O)CC(=O)OCC.FC(F)(F)C(F)(F)CCCI
C=CCCCCCC(=O)C(CCCC(F)(F)C(F)(F)F)C(=O)OCC
null
null
C1CCOC1
C-C Coupling
OtherReaction
eb3faf2a43700925ab4f46cf65072b7145e4e060dba25a917e6b7428f38e349e
61bad66347ae366bfd0a2cd3779dd3d0c29125e97564b97243e11258be3b2a9f
null
I-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[#8:5]-[C:6](=[O;D1;H0:7])-[CH2;D2;+0:8]-[C:9](-[C:10])=[O;D1;H0:11]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[CH;D3;+0:8](-[C:6](=[O;D1;H0:7])-[#8:5]-[C:4])-[C:9](-[C:10])=[O;D1;H0:11]
59
[{"value": 59.0, "product": "C(C)OC(C(C(CCCCCC=C)=O)CCCC(C(F)(F)F)(F)F)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
On the other hand, to a solution of 3-oxo-dec-9-enoic acid ethyl ester (4.32 g, 20.3 mmol) in THF (15 ml) at 0° C. was added potassium tert-butoxide (2.73 g, 24.3 mmol) This resulting mixture was stirred at room temperature under nitrogen for 30 min. The mixture of 4,4,5,5,5-pentafluoro-iodopentane was added and mixtur...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone
Ketone.Ester
null
null
null
HI
C1CCOC1
null
0.5
C=CCCCCCC(=O)CC(=O)OCC.FC(F)(F)C(F)(F)CCCI>C1CCOC1>C=CCCCCCC(=O)C(CCCC(F)(F)C(F)(F)F)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f7467f471bd84b2393713aa13d35d7c3
OCCCC(F)(F)C(F)(F)F>>O=C(O)CCC(F)(F)C(F)(F)F
CC(=O)C.OS(=O)(=O)O.O=[Cr](=O)=O.FC(CCCO)(C(F)(F)F)F>>FC(CCC(=O)O)(C(F)(F)F)F
[CH2:2]([OH:3])[CH2:4][CH2:5][C:6]([F:7])([F:8])[C:9]([F:10])([F:11])[F:12]>>[O:1]=[C:2]([OH:3])[CH2:4][CH2:5][C:6]([F:7])([F:8])[C:9]([F:10])([F:11])[F:12]
OCCCC(F)(F)C(F)(F)F
O=C(O)CCC(F)(F)C(F)(F)F
null
null
CC(=O)C
Oxidation
Oxidation of alcohol to carboxylic acid
b709baac44a995a9a8f6386a6b5d87f98c32eb5a0636340abc1f778fae827230
4454822e22dc2dc24e7495385256bfce456e337c240bb764261f81dbeda1aaa1
null
[C:1]-[C:2]-[CH2;D2;+0:3]-[O;D1;H1:4]>>[C:1]-[C:2]-[C;H0;D3;+0:3](=[O;D1;H0:5])-[O;D1;H1:4]
82.1
[{"value": 82.0, "product": "FC(CCC(=O)O)(C(F)(F)F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.1, "product": "FC(CCC(=O)O)(C(F)(F)F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a stirred solution of Jones reagent (20 ml, 160 mmol) in acetone (20 ml), cooled in an ice bath, a solution of 4,4,5,5,5-pentafluoro-1-pentanol (7.12 g, 40 mmol) in acetone (30 ml) was added dropwise. After remaining ice bath, the mixture was stirred continuously at room temperature for 1 h. The mixture was poured i...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Carboxylic acid
null
null
null
Other
CC(=O)C
null
1
OCCCC(F)(F)C(F)(F)F>CC(=O)C>O=C(O)CCC(F)(F)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c9a8b8dff5a04d489160160a139b1a41
CCOC(C)=O.O=C(Cl)CCC(F)(F)C(F)(F)F>>CCOC(=O)CC(=O)CCC(F)(F)C(F)(F)F
FC(CCC(=O)Cl)(C(F)(F)F)F.C(C)(=O)OCC.C[Si]([N-][Si](C)(C)C)(C)C.[Na+]>>FC(CCC(CC(=O)OCC)=O)(C(F)(F)F)F
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH3:6].Cl[C:7](=[O:8])[CH2:9][CH2:10][C:11]([F:12])([F:13])[C:14]([F:15])([F:16])[F:17]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:7](=[O:8])[CH2:9][CH2:10][C:11]([F:12])([F:13])[C:14]([F:15])([F:16])[F:17]
CCOC(C)=O.O=C(Cl)CCC(F)(F)C(F)(F)F
CCOC(=O)CC(=O)CCC(F)(F)C(F)(F)F
null
null
C1CCOC1
C-C Coupling
OtherReaction
9c255438d8e6adeba9ee52582b8e97af5f85bef382cd416953270ac55bd10486
4c7bc8856483317e0c04a17d8cd6aba13cdf5ed9f64b61fe01f230a819039f82
null
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C:5]-[#8:6]-[C:7](-[CH3;D1;+0:8])=[O;D1;H0:9]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH2;D2;+0:8]-[C:7](=[O;D1;H0:9])-[#8:6]-[C:5]
56
[{"value": 56.0, "product": "FC(CCC(CC(=O)OCC)=O)(C(F)(F)F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 55.7, "product": "FC(CCC(CC(=O)OCC)=O)(C(F)(F)F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a stirred solution of ethyl acetate enolate, prepared from ethyl acetate (4.4 g, 50 mmol) and sodium hexamethyldisilazide (50 mmol) in THF at −70° C., was added neat 4,4,5,5,5-pentafluoropentanoyl chloride (2.1 g, 10 mmol) at −70° C. Cooling bath was removed and the reaction mixture was allowed to warm to room tempe...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ester
Ketone
null
null
null
HCl
C1CCOC1
null
null
CCOC(C)=O.O=C(Cl)CCC(F)(F)C(F)(F)F>C1CCOC1>CCOC(=O)CC(=O)CCC(F)(F)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8f05e99b3c1f4ee294971c754d2bc47e
C=CCCCCCCBr.[I-]>>C=CCCCCCCI
BrCCCCCCC=C.[I-].[Na+]>>ICCCCCCC=C
Br[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=[CH2:1].[I-:9]>>[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][I:9]
C=CCCCCCCBr.[I-]
C=CCCCCCCI
null
null
CC(CC)=O
Functional Group Interconversion
OtherReaction
e944a2acb95a43a23818321f2ac2f96ba2f2b8d34f52c1cfd1e3802d2403177f
e2ca6f9fe1078a3836d617896a4e5cc310fb155ca459b021e2b549b3e61f1df7
null
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[I-;H0;D0:4]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[I;H0;D1;+0:4]
null
[]
null
null
null
null
A mixture of 8-bromo-1-octene (1.34 g, 7 mmol) and sodium iodide (5.25 g, 35 mmol) in 2-butanone (15 ml) was stirred under reflux for 1 h. The mixture was concentrated in vacuo to a half of its original volume and hexane and water was added. Organic layer was washed with 5% aqueous sodium thiosulfate, saturated sodium ...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Primary halide
null
null
null
Br-
CC(CC)=O
null
null
C=CCCCCCCBr.[I-]>CC(CC)=O>C=CCCCCCCI
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-126b46c583eb4d38b98c533b7ad86f3c
C=CCCCCCCI.CCOC(=O)CC(=O)CCC(F)(F)C(F)(F)F>>C=CCCCCCCC(C(=O)CCC(F)(F)C(F)(F)F)C(=O)OCC
FC(CCC(CC(=O)OCC)=O)(C(F)(F)F)F.[O-]CCCC.ICCCCCCC=C>>FC(CCC(=O)C(C(=O)OCC)CCCCCCC=C)(C(F)(F)F)F
I[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=[CH2:1].[CH2:9]([C:10](=[O:11])[CH2:12][CH2:13][C:14]([F:15])([F:16])[C:17]([F:18])([F:19])[F:20])[C:21](=[O:22])[O:23][CH2:24][CH3:25]>>[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH:9]([C:10](=[O:11])[CH2:12][CH2:13][C:14]([F:15])([F:16])[C:17]([F:18])([F...
C=CCCCCCCI.CCOC(=O)CC(=O)CCC(F)(F)C(F)(F)F
C=CCCCCCCC(C(=O)CCC(F)(F)C(F)(F)F)C(=O)OCC
null
null
[K].C1CCOC1
C-C Coupling
OtherReaction
eb3faf2a43700925ab4f46cf65072b7145e4e060dba25a917e6b7428f38e349e
61bad66347ae366bfd0a2cd3779dd3d0c29125e97564b97243e11258be3b2a9f
null
I-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[C:5](=[O;D1;H0:6])-[CH2;D2;+0:7]-[C:8](=[O;D1;H0:9])-[#8:10]-[C:11]>>[C:4]-[C:5](=[O;D1;H0:6])-[CH;D3;+0:7](-[CH2;D2;+0:1]-[C:2]-[C:3])-[C:8](=[O;D1;H0:9])-[#8:10]-[C:11]
null
[]
null
null
30
MINUTE
To a stirred solution of ethyl 6,6,7,7,7-pentafluoro-3-oxoheptanoate (262 mg, 1 mmol) in anhydrous THF (4 ml), potassium tret-butoxide (112 mg, 1 mmol) was added as a solid and the mixture was stirred at room temperature for 30 min. Then to a solution of 8-iodo-1-octene (357 mg, 1.5 mmol) in anhydrous THF (1 ml) was ad...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone
Ketone.Ester
null
null
null
HI
[K].C1CCOC1
null
0.5
C=CCCCCCCI.CCOC(=O)CC(=O)CCC(F)(F)C(F)(F)F>[K].C1CCOC1>C=CCCCCCCC(C(=O)CCC(F)(F)C(F)(F)F)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bba4881519bd4898a0f1cb168e48df4a
CCOC(=O)C(CCCCCCCCCC1c2ccc(OCOC)cc2OCC1(C)c1ccc(OCOC)cc1)C(=O)CCC(F)(F)C(F)(F)F>>CCOC(=O)C(CCCCCCCCCC1c2ccc(O)cc2OCC1(C)c1ccc(O)cc1)C(=O)CCC(F)(F)C(F)(F)F
FC(CCC(=O)C(C(=O)OCC)CCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC)(C(F)(F)F)F>>FC(CCC(=O)C(C(=O)OCC)CCCCCCCCCC1C(COC2=CC(=CC=C12)O)(C)C1=CC=C(C=C1)O)(C(F)(F)F)F
COC[O:21][c:20]1[cH:19][cH:18][c:17]2[c:23]([cH:22]1)[O:24][CH2:25][C:26]([CH3:27])([c:28]1[cH:29][cH:30][c:31]([O:32]COC)[cH:33][cH:34]1)[CH:16]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:35](=[O:36])[CH2:37][CH2:38][C:39]([F:40])([F:41])[C:42]([F:43...
CCOC(=O)C(CCCCCCCCCC1c2ccc(OCOC)cc2OCC1(C)c1ccc(OCOC)cc1)C(=O)CCC(F)(F)C(F)(F)F
CCOC(=O)C(CCCCCCCCCC1c2ccc(O)cc2OCC1(C)c1ccc(O)cc1)C(=O)CCC(F)(F)C(F)(F)F
null
Cl
C(C)(=O)OCC.C(C)O
Reduction
OtherReaction
ca434a15af04bd105d14de328e5decdefa40fa872c8bf2d8a06e38dd9d786610
9290d799ef03b273f5a33508bad8fca1206e009b9df18f946351c38e7647a04c
c1ccc(C2COc3ccccc3C2)cc1
C-O-C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].C-O-C-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]
null
[]
null
null
2.5
DAY
To a stirred solution of ethyl 2-(4,4,5,5,5-pentafluoro-1-oxopentyl)-11-[(3RS,4RS)-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman-4-yl]undecanoate (128 mg, 0.17 mmol) in ethyl alcohol (5 ml), was added concentrated aqueous hydrochloric acid (10 drops) at room temperature under N2 atmosphere. The mixture wa...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Ether
Aromatic alcohol.Aromatic alcohol
null
null
c1ccc2c(c1)CCCO2.c1ccccc1
HO-
Cl.C(C)(=O)OCC.C(C)O
null
60
CCOC(=O)C(CCCCCCCCCC1c2ccc(OCOC)cc2OCC1(C)c1ccc(OCOC)cc1)C(=O)CCC(F)(F)C(F)(F)F>Cl.C(C)(=O)OCC.C(C)O>CCOC(=O)C(CCCCCCCCCC1c2ccc(O)cc2OCC1(C)c1ccc(O)cc1)C(=O)CCC(F)(F)C(F)(F)F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5622d29f00734a1982d17b4dcd5b87fc
CCOC(=O)/C(=C/CCC(F)(F)C(F)(F)F)CCCCCCCCCC1c2ccc(OCOC)cc2OCC1(C)c1ccc(OCOC)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O)cc1
FC(CC/C=C(/C(=O)OCC)\CCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC)(C(F)(F)F)F.Cl>>FC(CC/C=C(/C(=O)O)\CCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC)(C(F)(F)F)F
CC[O:46][C:44](/[C:33]([CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH:23]1[C:9]([c:8]2[cH:7][cH:6][c:5]([O:4][CH2:3][O:2][CH3:1])[cH:48][cH:47]2)([CH3:10])[CH2:11][O:12][c:13]2[cH:14][c:15]([O:16][CH2:17][O:18][CH3:19])[cH:20][cH:21][c:22]21)=[CH:34]/[CH2:35][CH2:36][C:37]([F:38])([F:39])[C...
CCOC(=O)/C(=C/CCC(F)(F)C(F)(F)F)CCCCCCCCCC1c2ccc(OCOC)cc2OCC1(C)c1ccc(OCOC)cc1
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O)cc1
null
null
[OH-].[K+].C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(C2COc3ccccc3C2)cc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])/[C:4](-[C:5])=[C:6]/[C:7]>>[C:5]/[C:4](=[C:6]\[C:7])-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
null
[]
70
CELSIUS
5
HOUR
To a stirred solution of ethyl (E)-6,6,7,7,7-pentafluoro-2-{9-[(3RS,4RS)-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman-4-yl]nonyl}-2-h eptenoate (116 mg, 0.16 mmol) in ethyl alcohol (5 ml), 5 N aqueous potassium hydroxide solution was added and the mixture was stirred under N2 atmosphere at 70° C. for 5 h...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccc2c(c1)CCCO2
Other
[OH-].[K+].C(C)O
70
5
CCOC(=O)/C(=C/CCC(F)(F)C(F)(F)F)CCCCCCCCCC1c2ccc(OCOC)cc2OCC1(C)c1ccc(OCOC)cc1>[OH-].[K+].C(C)O>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-64820e20b2e1429798acad9ad3103b90
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O)cc1>>CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O
FC(CC/C=C(/C(=O)O)\CCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC)(C(F)(F)F)F>>FC(CC/C=C(/C(=O)O)\CCCCCCCCCC1C(COC2=CC(=CC=C12)O)(C)C1=CC=C(C=C1)O)(C(F)(F)F)F
COC[O:7][c:6]1[cH:5][cH:4][c:3]([C:2]2([CH3:1])[CH2:10][O:11][c:12]3[cH:13][c:14]([O:15]COC)[cH:16][cH:17][c:18]3[CH:19]2[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]/[C:29](=[CH:30]\[CH2:31][CH2:32][C:33]([F:34])([F:35])[C:36]([F:37])([F:38])[F:39])[C:40](=[O:41])[OH:42])[cH:9][cH:8]1>>[CH3:...
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O)cc1
CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O
null
Cl
O.C(C)O
Reduction
OtherReaction
ca434a15af04bd105d14de328e5decdefa40fa872c8bf2d8a06e38dd9d786610
9290d799ef03b273f5a33508bad8fca1206e009b9df18f946351c38e7647a04c
c1ccc(C2COc3ccccc3C2)cc1
C-O-C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].C-O-C-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]
null
[]
40
CELSIUS
6
HOUR
To a stirred solution of (E)-6,6,7,7,7-pentafluoro-2-{9-[(3RS,4RS)-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman-4-yl]nonyl}-2-heptenoic acid (111 mg, 0.16 mmol) in ethyl alcohol (5 ml), was added 6 N aqueous solution of hydrochloric acid (30 drops) and the reaction mixture was stirred at 40° C. for 6 h. ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Ether
Aromatic alcohol.Aromatic alcohol
null
null
c1ccccc1.c1ccc2c(c1)CCCO2
HO-
Cl.O.C(C)O
40
6
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O)cc1>Cl.O.C(C)O>CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1CCCCCCCCC/C(=C\CCC(F)(F)C(F)(F)F)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8a2c55af2e3b4a24ae2a63540a9262c5
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCCN)cc1.O=S(=O)(Cl)CCCC(F)(F)C(F)(F)F>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCCNCCCC(F)(F)C(F)(F)F)cc1
NCCCCCCCCCC1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC.FC(CCCS(=O)(=O)Cl)(C(F)(F)F)F.C(C)N(CC)CC>>COCOC1=CC=C2C(C(COC2=C1)(C)C1=CC=C(C=C1)OCOC)CCCCCCCCCNCCCC(C(F)(F)F)(F)F
[CH3:1][O:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8]([C:9]2([CH3:10])[CH2:11][O:12][c:13]3[cH:14][c:15]([O:16][CH2:17][O:18][CH3:19])[cH:20][cH:21][c:22]3[CH:23]2[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][NH2:33])[cH:44][cH:45]1.O=S(=O)(Cl)[CH2:34][CH2:35][CH2:36][C:37]([F:38])([F:39])[C:40]([F...
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCCN)cc1.O=S(=O)(Cl)CCCC(F)(F)C(F)(F)F
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCCNCCCC(F)(F)C(F)(F)F)cc1
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
OtherReaction
158f49fe57c7ac38d88fe4b2207dc19199f94508ccd68dac6442c76c103458a3
298452d0d798e9f10a3b6cebf52647f808001249292b5fe8eb23812442d1d9b8
c1ccc(C2COc3ccccc3C2)cc1
Cl-S(=O)(=O)-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[C:5]-[NH2;D1;+0:6]>>[C:4]-[C:5]-[NH;D2;+0:6]-[CH2;D2;+0:1]-[C:2]-[C:3]
73.8
[{"value": 67.0, "product": "COCOC1=CC=C2C(C(COC2=C1)(C)C1=CC=C(C=C1)OCOC)CCCCCCCCCNCCCC(C(F)(F)F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73.8, "product": "COCOC1=CC=C2C(C(COC2=C1)(C)C1=CC=C(C=C1)OCOC)CCCCCCCCCNCCCC(C(F)(F)F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
4-(9-aminononyl)-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman (82.3 mg, 0.17 mmol) was dissolved in 5 ml of methylenechloride under argon atmosphere, which was then cooled down to 0° C. 4,4,5,5,5-pentafluoropentylsulfonyl chloride (110.4 mg, 0.42 mmol) in 1 ml of methylene chloride and triethylamine (0.0...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Secondary amine
null
null
c1ccccc1.c1ccc2c(c1)CCCO2
HCl
C(Cl)Cl
0
0.5
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCCN)cc1.O=S(=O)(Cl)CCCC(F)(F)C(F)(F)F>C(Cl)Cl>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2CCCCCCCCCNCCCC(F)(F)C(F)(F)F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8f46b3be43a246868cb922f99a121180
O=Cc1ccc(Br)cc1.OCCO>>Brc1ccccc1C1COCO1
BrC1=CC=C(C=O)C=C1.C1(=CC=CC=C1)C.C(CO)O>>BrC1=C(C=CC=C1)C1OCOC1
[Br:1][c:2]1[cH:3][cH:4][c:7]([CH:8]=[O:12])[cH:6][cH:5]1.O[CH2:11][CH2:9][OH:10]>>[Br:1][c:2]1[cH:3][cH:4][cH:5][cH:6][c:7]1[CH:8]1[CH2:9][O:10][CH2:11][O:12]1
O=Cc1ccc(Br)cc1.OCCO
Brc1ccccc1C1COCO1
null
C1(=CC=C(C=C1)S(=O)(=O)O)C
null
Aromatic Heterocycle Formation
OtherReaction
76f52cb283311be0b4b9fa2854a03dd35110b89638a33866f31c5a381154af4e
06198f7e3e166c4884409e793066a85ca1d4434fe1fe7b176f53070242819939
c1ccc(C2COCO2)cc1
O-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[OH;D1;+0:3].[Br;D1;H0:4]-[c;H0;D3;+0:5]1:[c:6]:[cH;D2;+0:7]:[c;H0;D3;+0:8](-[CH;D2;+0:9]=[O;H0;D1;+0:10]):[c:11]:[cH;D2;+0:12]:1>>[Br;D1;H0:4]-[c;H0;D3;+0:5]1:[c:6]:[cH;D2;+0:7]:[cH;D2;+0:12]:[c:11]:[c;H0;D3;+0:8]:1-[CH;D3;+0:9]1-[CH2;D2;+0:2]-[O;H0;D2;+0:3]-[CH2;D2;+0:1]-[O;H0;D2;+0:10]-...
89
[{"value": 89.0, "product": "BrC1=C(C=CC=C1)C1OCOC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
In a round-bottomed flask equipped with a Dean Stark trap and a condenser, was added a solution of p-Bromobenzaldehyde (5 g, 27 mmol) in toluene (25 mL). To this mixture were then added p-toluenesulfonic acid (50 mg, 0.26 mmol) and etylene glycol (1.84 g, 29.7 mmol). The mixture was heated to reflux under nitrogen atmo...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aldehyde.Primary alcohol.Primary alcohol
Aromatic halide.Ether.Ether
c1ccccc1
c1ccccc1.C1COCO1
c1ccccc1.C1COCO1
HO-
C1(=CC=C(C=C1)S(=O)(=O)O)C
null
null
O=Cc1ccc(Br)cc1.OCCO>C1(=CC=C(C=C1)S(=O)(=O)O)C>Brc1ccccc1C1COCO1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7696eefa70854ec68278c2cac1e07693
CC(C)(C)[Si](C)(C)Cl.OCc1ccc(Br)cc1>>CC(C)(C)[Si](C)(C)OCc1ccc(Br)cc1
CO.[Si](C)(C)(C(C)(C)C)Cl.BrC1=CC=C(CO)C=C1.N1C=NC=C1>>BrC1=CC=C(CO[Si](C)(C)C(C)(C)C)C=C1
Cl[Si:5]([C:2]([CH3:1])([CH3:3])[CH3:4])([CH3:6])[CH3:7].[OH:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([Br:14])[cH:15][cH:16]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([CH3:6])([CH3:7])[O:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([Br:14])[cH:15][cH:16]1
CC(C)(C)[Si](C)(C)Cl.OCc1ccc(Br)cc1
CC(C)(C)[Si](C)(C)OCc1ccc(Br)cc1
null
null
CCCCCC.CN(C)C=O.C(C)(=O)OCC
Protection
Alcohol protection with silyl ethers
0085cd6629412592263fdf1537bdf8c19ef10dbeafe6f880807464d8107fa715
d2a170d01b2f3ec57d6fac058519475050ba5531f5d304635fb42e153d5bb9b5
c1ccccc1
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].[OH;D1;+0:8]-[C:9]-[c:10]>>[C;D1;H3:5]-[C:4](-[C;D1;H3:6])(-[C;D1;H3:7])-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[O;H0;D2;+0:8]-[C:9]-[c:10]
91
[{"value": 91.0, "product": "BrC1=CC=C(CO[Si](C)(C)C(C)(C)C)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.7, "product": "BrC1=CC=C(CO[Si](C)(C)C(C)(C)C)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of p-bromobenzyl alcohol (5.0 g, 26.7 mmol) in DMF (10 mL) was added imidazole (4.54 g, 66.7 mmol) followed by addition of tert-butyldimethylsilyl chloride (6.01 g, 40 mmol). The progress of the reaction was monitored by TLC. When the reaction was complete (about 2 h), methanol was added and diluted by 20...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Silyl protective group
TMS ether protective group
null
null
c1ccccc1
HCl
CCCCCC.CN(C)C=O.C(C)(=O)OCC
null
null
CC(C)(C)[Si](C)(C)Cl.OCc1ccc(Br)cc1>CCCCCC.CN(C)C=O.C(C)(=O)OCC>CC(C)(C)[Si](C)(C)OCc1ccc(Br)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b331bea50b8341399b359a762691f74c
BrBr.CN(CCO)c1ccccc1>>OCCNCc1ccc(Br)cc1
C(C)N(CC)CC.CN(C1=CC=CC=C1)CCO.CO.BrBr.C(C)(=O)OCC.BrBr>>BrC1=CC=C(C=C1)CNCCO
Br[Br:10].[OH:1][CH2:2][CH2:3][N:4]([CH3:5])[c:6]1[cH:7][cH:8][cH:9][cH:11][cH:12]1>>[OH:1][CH2:2][CH2:3][NH:4][CH2:5][c:6]1[cH:7][cH:8][c:9]([Br:10])[cH:11][cH:12]1
BrBr.CN(CCO)c1ccccc1
OCCNCc1ccc(Br)cc1
null
[Cl-].C(C)[N+](CC)(CC)CC
C(Cl)Cl
Functional Group Interconversion
OtherReaction
bffd665e61d49b1d6457692b10477c6250cf3ee2e1f8b0416172bde2b0bbdf7e
0a260d90fde2f27bcc20d80121977fbfb547a023e71819da383ff02783b8a0ac
c1ccccc1
Br-[Br;H0;D1;+0:1].[C:2]-[C:3]-[N;H0;D3;+0:4](-[CH3;D1;+0:5])-[c;H0;D3;+0:6]1:[c:7]:[c:8]:[cH;D2;+0:9]:[c:10]:[c:11]:1>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:9]1:[c:8]:[c:7]:[c;H0;D3;+0:6](-[CH2;D2;+0:5]-[NH;D2;+0:4]-[C:3]-[C:2]):[c:11]:[c:10]:1
75
[{"value": 35.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.0, "product": "BrC1=CC=C(C=C1)CNCCO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 2-(N-methylanilino)ethanol (0.76 g, 5 mmol) in methylene chloride (5 mL) were added tetraethylammonium chloride (83.0 mg, 0.5 mmol) and 0.1 mL of methanol. While stirring, a solution of bromine (0.8 g, 5 mmol) in methylene chloride (5 mL) was added slowly in a period of 5 minutes. When the color of the...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Aromatic halide.Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1
HBr
[Cl-].C(C)[N+](CC)(CC)CC.C(Cl)Cl
null
null
BrBr.CN(CCO)c1ccccc1>[Cl-].C(C)[N+](CC)(CC)CC.C(Cl)Cl>OCCNCc1ccc(Br)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-93791a264422479192af704bf0566f67
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2c2ccc(O[Si](C)(C)C(C)(C)C)cc2)cc1>>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2c2ccc(O)cc2)cc1
[Si](C)(C)(C(C)(C)C)OC1=CC=C(C=C1)C1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC.O>>OC1=CC=C(C=C1)C1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC
CC(C)(C)[Si](C)(C)[O:28][c:27]1[cH:26][cH:25][c:24]([CH:23]2[C:9]([c:8]3[cH:7][cH:6][c:5]([O:4][CH2:3][O:2][CH3:1])[cH:32][cH:31]3)([CH3:10])[CH2:11][O:12][c:13]3[cH:14][c:15]([O:16][CH2:17][O:18][CH3:19])[cH:20][cH:21][c:22]32)[cH:30][cH:29]1>>[CH3:1][O:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8]([C:9]2([CH3:10])[CH2:11][O:...
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2c2ccc(O[Si](C)(C)C(C)(C)C)cc2)cc1
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2c2ccc(O)cc2)cc1
null
null
O1CCCC1
Deprotection
Alcohol deprotection from silyl ethers
e70131badc7d7d580ed75b2dfb3ce6df2a5f496b2119611cf5354e1267babe73
b09ece7bccc3ff762f4ff5407ad846fffba6d6a63735853c86a86d29904f54ed
c1ccc(C2COc3ccccc3C2c2ccccc2)cc1
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
96.7
[{"value": 96.4, "product": "OC1=CC=C(C=C1)C1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.7, "product": "OC1=CC=C(C=C1)C1C(COC2=CC(=CC=C12)OCOC)(C)C1=CC=C(C=C1)OCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of (3RS,4RS)-4-[4-(t-butyldimethylsilyloxy)phenyl]-7-(methoxymethoxy)-3-[4-(methoxymethoxy)phenyl]-3-methylchroman (1.1 g, 1.99 mmol) in tetrabydrofuran (10 ml) was added 1N-tetrabutylainmoniumfluoride (3.99 ml, 3.99 mmol) in tetrahydrofuran and stirred at room temperature for 1 hour. After the reaction w...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Aromatic alcohol
null
null
c1ccccc1.c1ccc2c(c1)CCCO2.c1ccccc1
Other
O1CCCC1
null
1
COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2c2ccc(O[Si](C)(C)C(C)(C)C)cc2)cc1>O1CCCC1>COCOc1ccc(C2(C)COc3cc(OCOC)ccc3C2c2ccc(O)cc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f4d215045ecf4defbe0bf8cdee4ae013
CCOC(=O)C(CCCCOc1ccc(C2c3ccc(OCOC)cc3OCC2(C)c2ccc(OCOC)cc2)cc1)(CCCC(F)(F)C(F)(F)F)C(=O)OCC>>CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)C(=O)O)cc1
FC(CCCC(C(=O)OCC)(C(=O)OCC)CCCCOC1=CC=C(C=C1)C1C(COC2=CC(=CC=C12)OCOC)(C1=CC=C(C=C1)OCOC)C)(C(F)(F)F)F.[OH-].[K+].Cl>>OC1=CC=C2C(C(COC2=C1)(C)C1=CC=C(C=C1)O)C1=CC=C(OCCCCC(C(=O)O)CCCC(C(F)(F)F)(F)F)C=C1
CCOC(=O)[C:29]([CH2:28][CH2:27][CH2:26][CH2:25][O:24][c:23]1[cH:22][cH:21][c:20]([CH:19]2[C:2]([CH3:1])([c:3]3[cH:4][cH:5][c:6]([O:7]COC)[cH:8][cH:9]3)[CH2:10][O:11][c:12]3[cH:13][c:14]([O:15]COC)[cH:16][cH:17][c:18]32)[cH:44][cH:43]1)([CH2:30][CH2:31][CH2:32][C:33]([F:34])([F:35])[C:36]([F:37])([F:38])[F:39])[C:40](=[...
CCOC(=O)C(CCCCOc1ccc(C2c3ccc(OCOC)cc3OCC2(C)c2ccc(OCOC)cc2)cc1)(CCCC(F)(F)C(F)(F)F)C(=O)OCC
CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)C(=O)O)cc1
null
null
O.C(C)O
Reduction
OtherReaction
6fc58f7e34786a8c30482cd79af46100cfd1f07d1d5b945a432845d8fef6bcea
12f44de4c575550003c50f0c8cf10614449e1119b65f0c51a60883df20a320e1
c1ccc(C2COc3ccccc3C2c2ccccc2)cc1
C-C-O-C(=O)-[C;H0;D4;+0:1](-[C:2]-[C:3])(-[C:4]-[C:5])-[C:6](=[O;D1;H0:7])-[O;H0;D2;+0:8]-C-C.C-O-C-[O;H0;D2;+0:9]-[c:10](:[c:11]):[c:12].C-O-C-[O;H0;D2;+0:13]-[c:14](:[c:15]):[c:16]>>[C:3]-[C:2]-[CH;D3;+0:1](-[C:4]-[C:5])-[C:6](=[O;D1;H0:7])-[OH;D1;+0:8].[OH;D1;+0:9]-[c:10](:[c:11]):[c:12].[OH;D1;+0:13]-[c:14](:[c:15]...
121.2
[{"value": 121.2, "product": "OC1=CC=C2C(C(COC2=C1)(C)C1=CC=C(C=C1)O)C1=CC=C(OCCCCC(C(=O)O)CCCC(C(F)(F)F)(F)F)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of diethyl 2-(4,4,5,5,5-pentafluoropentyl)-2-(4-((3RS,4RS)-4-(3-methyl-7-(methyloxymethyloxy)-3-(4-(methyloxymethyloxy)phenyl)chroman-4-yl)phenyloxy)butyl)propane-1,3-dioate (0.552 g, 0.68 mmol) in ethanol (10 ml) was added the solution of potassium hydroxide (1.53 g, 27.23 mmol) in water (5 ml) and the m...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Ether.Ether.Ether.Ether
Carboxylic acid.Aromatic alcohol.Aromatic alcohol
null
null
c1ccccc1.c1ccc2c(c1)CCCO2.c1ccccc1
HO-
O.C(C)O
null
null
CCOC(=O)C(CCCCOc1ccc(C2c3ccc(OCOC)cc3OCC2(C)c2ccc(OCOC)cc2)cc1)(CCCC(F)(F)C(F)(F)F)C(=O)OCC>O.C(C)O>CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)C(=O)O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-92e5dcd1589c4ee4b4d85ade5225b0e3
CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)(C(=O)O)C(=O)O)cc1>>CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)C(=O)O)cc1
FC(CCCC(C(=O)O)(C(=O)O)CCCCOC1=CC=C(C=C1)C1C(COC2=CC(=CC=C12)O)(C)C1=CC=C(C=C1)O)(C(F)(F)F)F.[Na+].[Cl-]>>OC1=CC=C2C(C(COC2=C1)(C)C1=CC=C(C=C1)O)C1=CC=C(OCCCCC(C(=O)O)CCCC(C(F)(F)F)(F)F)C=C1
O=C(O)[C:29]([CH2:28][CH2:27][CH2:26][CH2:25][O:24][c:23]1[cH:22][cH:21][c:20]([CH:19]2[C:2]([CH3:1])([c:3]3[cH:4][cH:5][c:6]([OH:7])[cH:8][cH:9]3)[CH2:10][O:11][c:12]3[cH:13][c:14]([OH:15])[cH:16][cH:17][c:18]32)[cH:44][cH:43]1)([CH2:30][CH2:31][CH2:32][C:33]([F:34])([F:35])[C:36]([F:37])([F:38])[F:39])[C:40](=[O:41])...
CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)(C(=O)O)C(=O)O)cc1
CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)C(=O)O)cc1
null
null
CS(=O)C
Reduction
OtherReaction
1dcdb0afd061fc08423f0103da81d9d30c22c6dc8004c40ee82cae1f931e4d18
292164ffdf89eeb341ee9424f24084b252a703a26bb77721b558b0f8a8528c45
c1ccc(C2COc3ccccc3C2c2ccccc2)cc1
O-C(=O)-[C;H0;D4;+0:1](-[C:2]-[C:3])(-[C:4]-[C:5])-[C:6](=[O;D1;H0:7])-[O;D1;H1:8]>>[C:3]-[C:2]-[CH;D3;+0:1](-[C:4]-[C:5])-[C:6](=[O;D1;H0:7])-[O;D1;H1:8]
67.6
[{"value": 67.6, "product": "OC1=CC=C2C(C(COC2=C1)(C)C1=CC=C(C=C1)O)C1=CC=C(OCCCCC(C(=O)O)CCCC(C(F)(F)F)(F)F)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 67.6, "product": "OC1=CC=C2C(C(COC2=C1)(C)C1=CC=C(C=C1)O)C1=CC=C(OCCCCC(C(=O)O)CCCC(C(F)(F)F)(F)F)C=C1", "details": "CALCULATEDPERCENTYIELD", "is...
null
null
null
null
A solution of (4,4,5,5,5-pentafluoropentyl)(4-(4-(7-hydroxy-3-(4-hydroxyphenyl)-3-methylchroman-4-yl)phenyloxy)butyl)methane-1,1-dicarboxylic acid (0.19 g, 0.285 mmol) in dimethylsulfoxide (7.6 ml) was stirred at 125° C. for 3 hours. After the reaction was completed, the reaction mixture was treated with saturated NaCl...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
null
null
null
c1ccccc1.c1ccc2c(c1)CCCO2.c1ccccc1
Other
CS(=O)C
null
null
CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)(C(=O)O)C(=O)O)cc1>CS(=O)C>CC1(c2ccc(O)cc2)COc2cc(O)ccc2C1c1ccc(OCCCCC(CCCC(F)(F)C(F)(F)F)C(=O)O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-147e45d0a1ff43f18315a65df564fe69
CC(C)(C)[Si](C)(C)Cl.OCCCCCCCBr>>CC(C)(C)[Si](C)(C)OCCCCCCCBr
O.BrCCCCCCCO.N1C=NC=C1.[Si](C)(C)(C(C)(C)C)Cl>>[Si](C)(C)(C(C)(C)C)OCCCCCCCBr
Cl[Si:5]([C:2]([CH3:1])([CH3:3])[CH3:4])([CH3:6])[CH3:7].[OH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][Br:16]>>[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([CH3:6])([CH3:7])[O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][Br:16]
CC(C)(C)[Si](C)(C)Cl.OCCCCCCCBr
CC(C)(C)[Si](C)(C)OCCCCCCCBr
null
null
O1CCCC1
Protection
Alcohol protection with silyl ethers
0085cd6629412592263fdf1537bdf8c19ef10dbeafe6f880807464d8107fa715
d2a170d01b2f3ec57d6fac058519475050ba5531f5d304635fb42e153d5bb9b5
null
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: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]
72
[{"value": 72.0, "product": "[Si](C)(C)(C(C)(C)C)OCCCCCCCBr", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.0, "product": "[Si](C)(C)(C(C)(C)C)OCCCCCCCBr", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of 7-bromoheptanol (50 g, 25.6 mmole) and imidazole (4.2 g, 61.5 mmole) in dry tetrahydrofuran (80 ml) was added t-butyldimethylsilyl chloride (4.6 g, 30.8 mmole) dropwise during 1 hour at room temperature. Then the reaction mixture was stirred overnight at room temperature. When the reaction was complete...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Silyl protective group
TMS ether protective group
null
null
null
HCl
O1CCCC1
null
8
CC(C)(C)[Si](C)(C)Cl.OCCCCCCCBr>O1CCCC1>CC(C)(C)[Si](C)(C)OCCCCCCCBr
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-09abb0bcc34b4aab8e6936789d4ceded
CCOC(=O)C(CCCC(F)(F)C(F)(F)F)C(=O)OCC.ClCCCCCCBr>>CCOC(=O)C(CCCCCCCl)(CCCC(F)(F)C(F)(F)F)C(=O)OCC
O.BrCCCCCCCl.C(C)OC(C(C(=O)OCC)CCCC(C(F)(F)F)(F)F)=O.[H-].[Na+]>>C(C)OC(C(C(=O)OCC)(CCCC(C(F)(F)F)(F)F)CCCCCCCl)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:14][CH2:15][CH2:16][C:17]([F:18])([F:19])[C:20]([F:21])([F:22])[F:23])[C:24](=[O:25])[O:26][CH2:27][CH3:28].Br[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][Cl:13]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][Cl:13])([CH2:14][CH2:15][CH2...
CCOC(=O)C(CCCC(F)(F)C(F)(F)F)C(=O)OCC.ClCCCCCCBr
CCOC(=O)C(CCCCCCCl)(CCCC(F)(F)C(F)(F)F)C(=O)OCC
null
null
O1CCCC1
C-C Coupling
OtherReaction
8175b6573d6439ec7ccc45bf6b48843ab56b46dccfc6504384c4766d09f35cc7
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
null
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[C:5]-[CH;D3;+0:6](-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10])-[C:11](=[O;D1;H0:12])-[#8:13]-[C:14]>>[C:4]-[C:5]-[C;H0;D4;+0:6](-[CH2;D2;+0:1]-[C:2]-[C:3])(-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10])-[C:11](=[O;D1;H0:12])-[#8:13]-[C:14]
56
[{"value": 56.0, "product": "C(C)OC(C(C(=O)OCC)(CCCC(C(F)(F)F)(F)F)CCCCCCCl)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 55.5, "product": "C(C)OC(C(C(=O)OCC)(CCCC(C(F)(F)F)(F)F)CCCCCCCl)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of (4,4,5,5,5-pentafluoropentyl)malonic acid diethyl ester (1 g, 3.12 mmol) in tetrahydrofuran (15 ml) was added sodium hydride (175 mg, 4.37 mmol), which was then stirred for 30 min at rt. 1-Bromo-6-chlorohexane (0.7 ml, 4.68 mmol) was added to this reaction mixture and the reaction mixture was refluxed ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
null
null
null
HBr
O1CCCC1
null
0.5
CCOC(=O)C(CCCC(F)(F)C(F)(F)F)C(=O)OCC.ClCCCCCCBr>O1CCCC1>CCOC(=O)C(CCCCCCCl)(CCCC(F)(F)C(F)(F)F)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7d17d3645d6548c9873294a02e062c24
CCOC(=O)C(CCCCCCCl)(CCCC(F)(F)C(F)(F)F)C(=O)OCC.[I-]>>CCOC(=O)C(CCCCCCI)(CCCC(F)(F)C(F)(F)F)C(=O)OCC
O.C(C)OC(C(C(=O)OCC)(CCCC(C(F)(F)F)(F)F)CCCCCCCl)=O.[I-].[Na+]>>C(C)OC(C(C(=O)OCC)(CCCC(C(F)(F)F)(F)F)CCCCCCI)=O
Cl[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH2:14][CH2:15][CH2:16][C:17]([F:18])([F:19])[C:20]([F:21])([F:22])[F:23])[C:24](=[O:25])[O:26][CH2:27][CH3:28].[I-:13]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][I:13])([CH2:14][CH2:15][CH2...
CCOC(=O)C(CCCCCCCl)(CCCC(F)(F)C(F)(F)F)C(=O)OCC.[I-]
CCOC(=O)C(CCCCCCI)(CCCC(F)(F)C(F)(F)F)C(=O)OCC
null
null
CC(=O)C
Functional Group Interconversion
OtherReaction
e944a2acb95a43a23818321f2ac2f96ba2f2b8d34f52c1cfd1e3802d2403177f
e2ca6f9fe1078a3836d617896a4e5cc310fb155ca459b021e2b549b3e61f1df7
null
Cl-[CH2;D2;+0:1]-[C:2]-[C:3].[I-;H0;D0:4]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[I;H0;D1;+0:4]
89.4
[{"value": 89.0, "product": "C(C)OC(C(C(=O)OCC)(CCCC(C(F)(F)F)(F)F)CCCCCCI)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.4, "product": "C(C)OC(C(C(=O)OCC)(CCCC(C(F)(F)F)(F)F)CCCCCCI)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 6-chlorohexyl-(4,4,5,5,5-pentafluoropentyl)malonic acid diethyl ester (743 mg, 1.69 mmol) in acetone (5 ml) was added sodium iodide (761 mg, 5.08 mmol), which was then refluxed for 4 h. When the reaction was completed, water was added to the reaction mixture and extracted with ethyl acetate. Then, the ...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Primary halide
null
null
null
Other
CC(=O)C
null
null
CCOC(=O)C(CCCCCCCl)(CCCC(F)(F)C(F)(F)F)C(=O)OCC.[I-]>CC(=O)C>CCOC(=O)C(CCCCCCI)(CCCC(F)(F)C(F)(F)F)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f80513410356425d8f6b7c43ded5850e
CC(C)OB(OC(C)C)OC(C)C.Fc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1>>OB(O)c1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(F)cc1
B(OC(C)C)(OC(C)C)OC(C)C.C(CCC)[Li].BrC=1C(=NN(C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=C(C=C1)F.[Cl-].[NH4+]>>FC1=CC=C(C=C1)C1=NN(C=C1B(O)O)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1
CC(C)O[B:2]([O:1]C(C)C)[O:3]C(C)C.Br[c:4]1[cH:5][n:6]([C:7]([c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)([c:14]2[cH:15][cH:16][cH:17][cH:18][cH:19]2)[c:20]2[cH:21][cH:22][cH:23][cH:24][cH:25]2)[n:26][c:27]1-[c:28]1[cH:29][cH:30][c:31]([F:32])[cH:33][cH:34]1>>[OH:1][B:2]([OH:3])[c:4]1[cH:5][n:6]([C:7]([c:8]2[cH:9][cH:10][...
CC(C)OB(OC(C)C)OC(C)C.Fc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1
OB(O)c1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(F)cc1
null
null
O1CCCC1.O.CCCCCC
Miscellaneous
Preparation of boronic acids
3844510e1842c6edc8fafe6b1abc924cfc5e60e61202cd5af68f36b3305fbec1
dafd25fbe01879c365f8c874026e570f49824f4bb82016b29d0c5d21aeb58ca3
c1ccc(-c2ccn(C(c3ccccc3)(c3ccccc3)c3ccccc3)n2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3](-[C:4]):[#7;a:5]:[c:6]:1-[c:7].C-C(-C)-O-[B;H0;D3;+0:8](-[O;H0;D2;+0:9]-C(-C)-C)-[O;H0;D2;+0:10]-C(-C)-C>>[C:4]-[#7;a:3]1:[#7;a:5]:[c:6](-[c:7]):[c;H0;D3;+0:1](-[B;H0;D3;+0:8](-[OH;D1;+0:9])-[OH;D1;+0:10]):[c:2]:1
null
[]
0
CELSIUS
30
MINUTE
47.5 g 4-bromo-3-(4-fluorophenyl)-1-trityl-1H-pyrazole was dissolved in 400 mL anhydrous tetrahydrofuran, and then 40.7 mL solution of 1.6 M n-butyl lithium in hexane was added dropwise thereto at −70° C. The mixture was stirred for 30 minutes, 17.2 mL triisopropyl borate was added dropwise thereto, and the mixture was...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Boronic acid
c1cn[nH]c1
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HBr
O1CCCC1.O.CCCCCC
0
0.5
CC(C)OB(OC(C)C)OC(C)C.Fc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1>O1CCCC1.O.CCCCCC>OB(O)c1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e067988a14f641bf928dd0855ddf7da7
CC(C)OB(OC(C)C)OC(C)C.N#Cc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2I)cc1>>N#Cc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2B(O)O)cc1
[Cl-].[NH4+].C(C)(C)[Mg]Br.IC=1C(=NN(C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=C(C#N)C=C1.B(OC(C)C)(OC(C)C)OC(C)C>>C(#N)C1=CC=C(C=C1)C1=NN(C=C1B(O)O)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1
CC(C)O[B:31]([O:32]C(C)C)[O:33]C(C)C.I[c:30]1[c:7](-[c:6]2[cH:5][cH:4][c:3]([C:2]#[N:1])[cH:35][cH:34]2)[n:8][n:9]([C:10]([c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[cH:29]1>>[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[n:8][n:9]([C...
CC(C)OB(OC(C)C)OC(C)C.N#Cc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2I)cc1
N#Cc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2B(O)O)cc1
null
null
O1CCCC1
Miscellaneous
OtherReaction
976aa5a00df0539fe32ca1f676305423435df099e4ae744398549c49ada58b5c
dafd25fbe01879c365f8c874026e570f49824f4bb82016b29d0c5d21aeb58ca3
c1ccc(-c2ccn(C(c3ccccc3)(c3ccccc3)c3ccccc3)n2)cc1
C-C(-C)-O-[B;H0;D3;+0:1](-[O;H0;D2;+0:2]-C(-C)-C)-[O;H0;D2;+0:3]-C(-C)-C.I-[c;H0;D3;+0:4]1:[c:5]:[#7;a:6](-[C:7]):[#7;a:8]:[c:9]:1-[c:10]>>[C:7]-[#7;a:6]1:[#7;a:8]:[c:9](-[c:10]):[c;H0;D3;+0:4](-[B;H0;D3;+0:1](-[OH;D1;+0:2])-[OH;D1;+0:3]):[c:5]:1
null
[]
null
null
30
MINUTE
17.2 mL of 0.75 M isopropyl magnesium bromide was added dropwise at −40° C. into a solution of 6 g 4-(4-iodo-1-trityl-1H-3-pyrazolyl)benzonitrile in tetrahydrofuran, and the mixture was stirred for 30 minutes. Subsequently, 3.3 mL triisopropyl borate was added dropwise thereto at −40° C. ad stirred at −10° C. for 2 hou...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Boronic acid
c1c[nH]nc1
c1c[nH]nc1
c1ccccc1.c1c[nH]nc1.c1ccccc1.c1ccccc1.c1ccccc1
HI
O1CCCC1
null
0.5
CC(C)OB(OC(C)C)OC(C)C.N#Cc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2I)cc1>O1CCCC1>N#Cc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2B(O)O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-11e0cb72b6b940c093fc6fa91043590f
Brc1ccc2nccn2c1.OB(O)c1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(F)cc1>>Fc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3nccn3c2)cc1
BrC=1C=CC=2N(C1)C=CN2.FC1=CC=C(C=C1)C1=NN(C=C1B(O)O)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.C(C)O.C([O-])([O-])=O.[Na+].[Na+]>>FC1=CC=C(C=C1)C1=NN(C=C1C=1C=CC=2N(C1)C=CN2)C(C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2
Br[c:30]1[cH:31][cH:32][c:33]2[n:34][cH:35][cH:36][n:37]2[cH:38]1.OB(O)[c:29]1[c:6](-[c:5]2[cH:4][cH:3][c:2]([F:1])[cH:40][cH:39]2)[n:7][n:8]([C:9]([c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)([c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[c:22]2[cH:23][cH:24][cH:25][cH:26][cH:27]2)[cH:28]1>>[F:1][c:2]1[cH:3][cH:4][c:5](...
Brc1ccc2nccn2c1.OB(O)c1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(F)cc1
Fc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3nccn3c2)cc1
null
null
C1(=CC=CC=C1)C.C(C)(=O)OCC
C-C Coupling
Suzuki coupling with boronic acids
608f2ba96b58fcb8873cdb9afc2c5161844f5a23b41ffec02067329cf10e0c19
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3nccn3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]2:[#7;a:5]:[c:6]:[c:7]:[#7;a:8]:2:[c:9]:1.O-B(-O)-[c;H0;D3;+0:10]1:[c:11]:[#7;a:12](-[C:13]):[#7;a:14]:[c:15]:1-[c:16]>>[C:13]-[#7;a:12]1:[#7;a:14]:[c:15](-[c:16]):[c;H0;D3;+0:10](-[c;H0;D3;+0:1]2:[c:2]:[c:3]:[c:4]3:[#7;a:5]:[c:6]:[c:7]:[#7;a:8]:3:[c:9]:2):[c:11]:1
80
[{"value": 80.0, "product": "FC1=CC=C(C=C1)C1=NN(C=C1C=1C=CC=2N(C1)C=CN2)C(C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2.2 g 6-bromoimidazo[1,2-a]pyridine, 6 g 3-(4-fluorophenyl)-1-trityl-1H-4-pyrazolylboronic acid (compound in Production Example 25), and 647 mg tetrakistriphenyl phosphine palladium were heated in a solution mixture of 30 mL ethanol, 30 mL toluene and 17 mL of 2 N aqueous sodium carbonate at 80° C. for 2 hours in a str...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccn2ccnc2c1.c1c[nH]nc1
c1c[nH]nc1.c1ccn2ccnc2c1
c1ccccc1.c1c[nH]nc1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccn2ccnc2c1
HBr.B
C1(=CC=CC=C1)C.C(C)(=O)OCC
null
null
Brc1ccc2nccn2c1.OB(O)c1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(F)cc1>C1(=CC=CC=C1)C.C(C)(=O)OCC>Fc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3nccn3c2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0e4d0ba3a8134211880ae0d64a80913e
CSc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3ncc(I)n3c2)cc1>>CS(=O)(=O)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3ncc(I)n3c2)cc1
O.IC1=CN=C2N1C=C(C=C2)C=2C(=NN(C2)C(C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C2=CC=C(C=C2)SC.OOS(=O)[O-].[K+]>>IC1=CN=C2N1C=C(C=C2)C=2C(=NN(C2)C(C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C2=CC=C(C=C2)S(=O)(=O)C
[CH3:1][S:2][c:5]1[cH:6][cH:7][c:8](-[c:9]2[n:10][n:11]([C:12]([c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)([c:19]3[cH:20][cH:21][cH:22][cH:23][cH:24]3)[c:25]3[cH:26][cH:27][cH:28][cH:29][cH:30]3)[cH:31][c:32]2-[c:33]2[cH:34][cH:35][c:36]3[n:37][cH:38][c:39]([I:40])[n:41]3[cH:42]2)[cH:43][cH:44]1>>[CH3:1][S:2](=[O:3])(...
CSc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3ncc(I)n3c2)cc1
CS(=O)(=O)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3ncc(I)n3c2)cc1
null
null
O1CCCC1.CO
Oxidation
OtherReaction
20dd6d48007b4fe7cd760226f21413eb5e71e6468db112596c2e7ea4858c8ac1
5cedc1bf0f43f21d78a249521ecfcec19fc5ac4895c41eed0e84f0c2618149fa
c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3nccn3c2)cc1
[C;D1;H3:1]-[S;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[C;D1;H3:1]-[S;H0;D4;+0:2](=[O;D1;H0:6])(=[O;D1;H0:7])-[c:3](:[c:4]):[c:5]
null
[]
null
null
2
HOUR
1.7 g 3-iodo-6-{3-[4-(methylsulfanyl)phenyl]-1-trityl-1H-4-pyrazolyl}imidazo[1,2-a]pyridine obtained in Example 42 was dissolved in a solvent mixture of 30 mL tetrahydrofuran and 30 mL methanol, and then 20 mL aqueous solution of 3.1 g oxone was added in divided portions thereto. The mixture was stirred at room tempera...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfone
null
null
c1ccccc1.c1c[nH]nc1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccn2ccnc2c1
null
O1CCCC1.CO
null
2
CSc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3ncc(I)n3c2)cc1>O1CCCC1.CO>CS(=O)(=O)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3ncc(I)n3c2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-91676370c4b44065a709dbf40d068486
Brc1ccc2nccn2c1.O=C1CCC(=O)N1I>>Brc1ccc2ncc(I)n2c1
S(=S)(=O)([O-])[O-].[Na+].[Na+].IN1C(CCC1=O)=O.BrC=1C=CC=2N(C1)C=CN2.O>>BrC=1C=CC=2N(C1)C(=CN2)I
[Br:1][c:2]1[cH:3][cH:4][c:5]2[n:6][cH:7][cH:8][n:10]2[cH:11]1.O=C1CCC(=O)N1[I:9]>>[Br:1][c:2]1[cH:3][cH:4][c:5]2[n:6][cH:7][c:8]([I:9])[n:10]2[cH:11]1
Brc1ccc2nccn2c1.O=C1CCC(=O)N1I
Brc1ccc2ncc(I)n2c1
null
null
CN(C=O)C
Functional Group Interconversion
OtherReaction
4574e733f80d194ce9380df52b6f0165984d072a1369f9c636a5ef16f4be8d67
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccn2ccnc2c1
O=C1-C-C-C(=O)-N-1-[I;H0;D1;+0:1].[c:2]:[#7;a:3]1:[cH;D2;+0:4]:[c:5]:[#7;a:6]:[c:7]:1:[c:8]>>[I;H0;D1;+0:1]-[c;H0;D3;+0:4]1:[c:5]:[#7;a:6]:[c:7](:[c:8]):[#7;a:3]:1:[c:2]
91.5
[{"value": 91.5, "product": "BrC=1C=CC=2N(C1)C(=CN2)I", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
10.7 g N-iodosuccinimide was added in divided portions to 100 mL solution of 9 g 6-bromoimidazo[1,2-a]pyridine in N,N-dimethylformamide, and the mixture was stirred for 2 hours. An aqueous sodium thiosulfate solution was added thereto and stirred for 1 hour, water was added thereto, and the formed crystals were collect...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1ccn2ccnc2c1.C1CCNC1
c1ccn2ccnc2c1
c1ccn2ccnc2c1
HO-
CN(C=O)C
null
2
Brc1ccc2nccn2c1.O=C1CCC(=O)N1I>CN(C=O)C>Brc1ccc2ncc(I)n2c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bdd0da86c2d84590b4e49a37136c4830
Brc1ccc2ncc(I)n2c1.COc1ccc(B(O)O)cc1>>COc1ccc(-c2cnc3ccc(Br)cn23)cc1
C(CCO)O.COC1=CC=C(C=C1)B(O)O.BrC=1C=CC=2N(C1)C(=CN2)I.P(=O)([O-])([O-])[O-].[K+].[K+].[K+]>>BrC=1C=CC=2N(C1)C(=CN2)C2=CC=C(C=C2)OC
I[c:7]1[cH:8][n:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][n:16]12.OB(O)[c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:18][cH:17]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][n:9][c:10]3[cH:11][cH:12][c:13]([Br:14])[cH:15][n:16]23)[cH:17][cH:18]1
Brc1ccc2ncc(I)n2c1.COc1ccc(B(O)O)cc1
COc1ccc(-c2cnc3ccc(Br)cn23)cc1
null
null
CN(C=O)C.C(C)OCC
C-C Coupling
Suzuki coupling with boronic acids
6d2f92e38cbc7faf246cda8a4b8669001b5c18f23ff87160bd75535916dab019
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cnc3ccccn23)cc1
I-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4](:[c:5]):[#7;a:6]:1:[c:7].O-B(-O)-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]>>[c:5]:[c:4]1:[#7;a:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]):[#7;a:6]:1:[c:7]
78.9
[{"value": 78.9, "product": "BrC=1C=CC=2N(C1)C(=CN2)C2=CC=C(C=C2)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
0.81 mL 1,3-propane diol was added to a suspension of 1.69 g 4-methoxyphenylboronic acid in 15 mL diethyl ether, and the mixture was stirred a room temperature for 1 hour. Formed water was removed, and the organic solvent was evaporated, whereby an oil was obtained. 2.7 g 6-bromo-3-iodoimidazo[1,2-a]pyridine (compound ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccn2ccnc2c1.c1ccccc1
c1ccccc1.c1ccn2ccnc2c1
c1ccccc1.c1ccn2ccnc2c1
HI.B
CN(C=O)C.C(C)OCC
null
1
Brc1ccc2ncc(I)n2c1.COc1ccc(B(O)O)cc1>CN(C=O)C.C(C)OCC>COc1ccc(-c2cnc3ccc(Br)cn23)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-87ea1ccdc5514c38a6a2a4a05e08cb86
Brc1ccc2ncc(I)n2c1.COC(=O)c1ccc(B2OC(C)(C)C(C)(C)O2)cc1>>COC(=O)c1ccc(-c2cnc3ccc(Br)cn23)cc1
BrC=1C=CC=2N(C1)C(=CN2)I.P(=O)([O-])([O-])[O-].[K+].[K+].[K+].CC1(OB(OC1(C)C)C1=CC=C(C(=O)OC)C=C1)C>>BrC=1C=CC=2N(C1)C(=CN2)C2=CC=C(C(=O)OC)C=C2
I[c:9]1[cH:10][n:11][c:12]2[cH:13][cH:14][c:15]([Br:16])[cH:17][n:18]12.CC1(C)OB([c:8]2[cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:20][cH:19]2)OC1(C)C>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8](-[c:9]2[cH:10][n:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][n:18]23)[cH:19][cH:20]1
Brc1ccc2ncc(I)n2c1.COC(=O)c1ccc(B2OC(C)(C)C(C)(C)O2)cc1
COC(=O)c1ccc(-c2cnc3ccc(Br)cn23)cc1
null
null
CN(C=O)C
C-C Coupling
Suzuki coupling with boronic esters
dcda447711556696a2b0cc312b40d9049503597a5d54a34fea6736b791985a24
b42efb3b6a7742d5af594c6a3031e487327e58e9f8c2f428ee68996c98377910
c1ccc(-c2cnc3ccccn23)cc1
C-C1(-C)-O-B(-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5])-O-C-1(-C)-C.I-[c;H0;D3;+0:6]1:[c:7]:[#7;a:8]:[c:9](:[c:10]):[#7;a:11]:1:[c:12]>>[c:10]:[c:9]1:[#7;a:8]:[c:7]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[#7;a:11]:1:[c:12]
67.8
[{"value": 67.8, "product": "BrC=1C=CC=2N(C1)C(=CN2)C2=CC=C(C(=O)OC)C=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2.3 g methyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate prepared according to T. Ishiyama et al., J. Org. Chem., 60, 7508 (1995), 2.0 g 6-bromo-3-iodoimidazo[1,2-a]pyridine (compound in Production Example 49), 2.5 g potassium phosphate, 360 mg tetrakistriphenyl phosphine palladium and 30 mL N,N-dimethylfor...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic ester
null
c1ccn2ccnc2c1.B1OCCO1.c1ccccc1
c1ccccc1.c1ccn2ccnc2c1
c1ccccc1.c1ccn2ccnc2c1
HI.B
CN(C=O)C
null
null
Brc1ccc2ncc(I)n2c1.COC(=O)c1ccc(B2OC(C)(C)C(C)(C)O2)cc1>CN(C=O)C>COC(=O)c1ccc(-c2cnc3ccc(Br)cn23)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0ca7047a8a154fe59d87a77e0f61519f
Nc1cc(Br)ccc1[N+](=O)[O-].S=C=S>>Sc1nc2ccc(Br)cc2[nH]1
BrC=1C=CC(=C(N)C1)[N+](=O)[O-].C(=S)=S.[OH-].[K+].O>>BrC=1C=CC2=C(NC(=N2)S)C1
O=[N+:3]([O-])[c:4]1[cH:5][cH:6][c:7]([Br:8])[cH:9][c:10]1[NH2:11].S=[C:2]=[S:1]>>[SH:1][c:2]1[n:3][c:4]2[cH:5][cH:6][c:7]([Br:8])[cH:9][c:10]2[nH:11]1
Nc1cc(Br)ccc1[N+](=O)[O-].S=C=S
Sc1nc2ccc(Br)cc2[nH]1
null
null
C(C)(=O)O.CO.C(C)O
Aromatic Heterocycle Formation
OtherReaction
c2c29974f4b5be07c21486a5b198dab3d77dbe80b212fcca89a8c66a9fb55acd
ecf3fe2b0af561b8897dfd28d098c701162f656ce0345b917de68408521bab59
c1ccc2[nH]cnc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4](-[NH2;D1;+0:5]):[c:6].S=[C;H0;D2;+0:7]=[S;H0;D1;+0:8]>>[SH;D1;+0:8]-[c;H0;D3;+0:7]1:[n;H0;D2;+0:1]:[c:2](:[c:3]):[c:4](:[c:6]):[nH;D2;+0:5]:1
null
[]
null
null
null
null
6.7 g of 4-bromo-1,2-benzenediamine obtained by reducing 5-bromo-2-nitroaniline was dissolved in 50 mL methanol, then 4.4 mL carbon disulfide was added thereto, a solution of 1.3 g potassium hydroxide in 40 mL ethanol was added little by little thereto, and the mixture was heated for 3.5 hours under reflux. The reactio...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Primary amine
Aromatic thiol
c1ccccc1
c1ccc2[nH]cnc2c1
c1ccc2[nH]cnc2c1
Other
C(C)(=O)O.CO.C(C)O
null
null
Nc1cc(Br)ccc1[N+](=O)[O-].S=C=S>C(C)(=O)O.CO.C(C)O>Sc1nc2ccc(Br)cc2[nH]1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6487d75bc2b74dfa990fbea3b98399e4
CCSc1nc2ccc(Br)cc2n1COC(=O)C(C)(C)C>>CCSc1nc2ccc(Br)cc2[nH]1
C(C(C)(C)C)(=O)OCN1C(=NC2=C1C=C(C=C2)Br)SCC.C(C(C)(C)C)(=O)OCN1C(=NC2=C1C=CC(=C2)Br)SCC>>BrC=1C=CC2=C(NC(=N2)SCC)C1
CC(C)(C)C(=O)OC[n:13]1[c:4]([S:3][CH2:2][CH3:1])[n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][c:12]21>>[CH3:1][CH2:2][S:3][c:4]1[n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][c:12]2[nH:13]1
CCSc1nc2ccc(Br)cc2n1COC(=O)C(C)(C)C
CCSc1nc2ccc(Br)cc2[nH]1
null
null
null
Reduction
OtherReaction
5e0e8f5be04754a5d1256a4b21b46ea8a49e71232936a58e92fcccb42ba1ebb2
b8e5da8ea19c403a2e974791a9cf591400749acb6b71151717aaece4f3b22bef
c1ccc2[nH]cnc2c1
C-C(-C)(-C)-C(=O)-O-C-[n;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:1-[#16:8]>>[#16:8]-[c:7]1:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[nH;D2;+0:1]:1
null
[]
null
null
null
null
11.8 g mixture of [6-bromo-2-(ethylsulfanyl)-1H-benzo[d]imidazol-1-yl]methyl pivalate and [5-bromo-2-(ethylsulfanyl)-1H-benzo[d]imidazol-1-yl]methyl pivalate in a ratio of 1:1 was obtained as pale yellow solid by the same method as in Production Example 64 from 8.1 g 6-bromo-2-(ethylsulfanyl)-1H-benzo[d]imidazole obtai...
10.6084/m9.figshare.5104873.v1
null
Ester
null
c1ccc2nc[nH]c2c1
c1ccc2[nH]cnc2c1
c1ccc2[nH]cnc2c1
HO-
null
null
null
CCSc1nc2ccc(Br)cc2n1COC(=O)C(C)(C)C>>CCSc1nc2ccc(Br)cc2[nH]1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-826001f3bb384ba3ae1349f678af87ac
CN1CCNCC1.Clc1ccnc2ccc(Br)cc12>>CN1CCN(c2ccnc3ccc(Br)cc23)CC1
BrC=1C=C2C(=CC=NC2=CC1)Cl.CN1CCNCC1.C([O-])([O-])=O.[K+].[K+].CN(C=O)C>>BrC=1C=C2C(=CC=NC2=CC1)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][NH:5][CH2:17][CH2:18]1.Cl[c:6]1[cH:7][cH:8][n:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]12>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][n:9][c:10]3[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]23)[CH2:17][CH2:18]1
CN1CCNCC1.Clc1ccnc2ccc(Br)cc12
CN1CCN(c2ccnc3ccc(Br)cc23)CC1
null
null
O.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
9f69c5c4a4ea31f8d76ec3987be7bd40b9cb34092e5d3f4fe2f7075ca0afa5f4
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(N3CCNCC3)ccnc2c1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[#7:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[c:6]:[c:5]1:[#7;a:4]:[c:3]:[c:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:12]2-[C:11]-[C:10]-[#7:9]-[C:14]-[C:13]-2):[c:7]:1:[c:8]
null
[]
130
CELSIUS
8
HOUR
A mixture of 485 mg 6-bromo-4-chloroquinoline, 1.1 mL N-methyl piperazine, 415 mg potassium carbonate and 10 mL N,N-dimethylformamide was stirred at 130° C. for 8 hours. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated. The organic layer was washed with water and brine an...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1C[NH]CCN1.c1ccc2ncccc2c1
C1C[NH]CC[NH]1.c1ccc2ncccc2c1
C1C[NH]CC[NH]1.c1ccc2ncccc2c1
HCl
O.C(C)(=O)OCC
130
8
CN1CCNCC1.Clc1ccnc2ccc(Br)cc12>O.C(C)(=O)OCC>CN1CCN(c2ccnc3ccc(Br)cc23)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a1988d1ba7504d79b97782eddbccf622
C1COCCN1.Clc1ccnc2ccc(Br)cc12>>Brc1ccc2nccc(N3CCOCC3)c2c1
BrC=1C=C2C(=CC=NC2=CC1)Cl.N1CCOCC1>>BrC=1C=C2C(=CC=NC2=CC1)N1CCOCC1
[NH:10]1[CH2:11][CH2:12][O:13][CH2:14][CH2:15]1.Cl[c:9]1[cH:8][cH:7][n:6][c:5]2[cH:4][cH:3][c:2]([Br:1])[cH:17][c:16]21>>[Br:1][c:2]1[cH:3][cH:4][c:5]2[n:6][cH:7][cH:8][c:9]([N:10]3[CH2:11][CH2:12][O:13][CH2:14][CH2:15]3)[c:16]2[cH:17]1
C1COCCN1.Clc1ccnc2ccc(Br)cc12
Brc1ccc2nccc(N3CCOCC3)c2c1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
7aa932588efc8aa136efe0e43f3ce3bc189e51460b145a5586838f54c5c09e43
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(N3CCOCC3)ccnc2c1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[#8:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[c:8]:[c:7]1:[c:5](:[c:6]):[#7;a:4]:[c:3]:[c:2]:[c;H0;D3;+0:1]:1-[N;H0;D3;+0:12]1-[C:11]-[C:10]-[#8:9]-[C:14]-[C:13]-1
null
[]
null
null
null
null
122 mg 6-bromo-4-chloroquinoline and 0.13 mL morpholine were reacted by the same method as in Production Example 74 to give 68 mg of the title compound as a colorless oil. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1COCCN1.c1ccc2ncccc2c1
c1ccc2ncccc2c1.C1COCC[NH]1
c1ccc2ncccc2c1.C1COCC[NH]1
HCl
null
null
null
C1COCCN1.Clc1ccnc2ccc(Br)cc12>>Brc1ccc2nccc(N3CCOCC3)c2c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9f5c47e6abf24ea29759758b6122ce6b
Clc1ccnc2ccc(Br)cc12.c1ccc(N2CCNCC2)nc1>>Brc1ccc2nccc(N3CCN(c4ccccn4)CC3)c2c1
BrC=1C=C2C(=CC=NC2=CC1)Cl.N1=C(C=CC=C1)N1CCNCC1>>BrC=1C=C2C(=CC=NC2=CC1)N1CCN(CC1)C1=NC=CC=C1
Cl[c:9]1[cH:8][cH:7][n:6][c:5]2[cH:4][cH:3][c:2]([Br:1])[cH:23][c:22]21.[NH:10]1[CH2:11][CH2:12][N:13]([c:14]2[cH:15][cH:16][cH:17][cH:18][n:19]2)[CH2:20][CH2:21]1>>[Br:1][c:2]1[cH:3][cH:4][c:5]2[n:6][cH:7][cH:8][c:9]([N:10]3[CH2:11][CH2:12][N:13]([c:14]4[cH:15][cH:16][cH:17][cH:18][n:19]4)[CH2:20][CH2:21]3)[c:22]2[cH:...
Clc1ccnc2ccc(Br)cc12.c1ccc(N2CCNCC2)nc1
Brc1ccc2nccc(N3CCN(c4ccccn4)CC3)c2c1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
98c8ae975f310a76e6895ad2c03786dcf0895f15908d93475fb9e11cf83466fa
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc(N2CCN(c3ccnc4ccccc34)CC2)nc1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[#7:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[c:8]:[c:7]1:[c:5](:[c:6]):[#7;a:4]:[c:3]:[c:2]:[c;H0;D3;+0:1]:1-[N;H0;D3;+0:12]1-[C:11]-[C:10]-[#7:9]-[C:14]-[C:13]-1
null
[]
null
null
null
null
291 mg 6-bromo-4-chloroquinoline and 0.91 mL 4-(2-pyridyl)piperazine were reacted by the same method as in Production Example 74 to give 373 mg of the title compound as a colorless oil. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
c1ccc2ncccc2c1.C1CNCC[NH]1
c1ccc2ncccc2c1.C1C[NH]CC[NH]1
c1ccc2ncccc2c1.C1C[NH]CC[NH]1.c1ccncc1
HCl
null
null
null
Clc1ccnc2ccc(Br)cc12.c1ccc(N2CCNCC2)nc1>>Brc1ccc2nccc(N3CCN(c4ccccn4)CC3)c2c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-27070b7657314989abb352220f1b84f4
CC(C)(C)OC(=O)N1CCNCC1.Clc1ccnc2ccc(Br)cc12>>CC(C)(C)OC(=O)N1CCN(c2ccnc3ccc(Br)cc23)CC1
BrC=1C=C2C(=CC=NC2=CC1)Cl.N1(CCNCC1)C(=O)OC(C)(C)C.C(C)N(CC)CC.CS(=O)C>>BrC=1C=C2C(=CC=NC2=CC1)N1CCN(CC1)C(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][NH:11][CH2:23][CH2:24]1.Cl[c:12]1[cH:13][cH:14][n:15][c:16]2[cH:17][cH:18][c:19]([Br:20])[cH:21][c:22]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[cH:13][cH:14][n:15][c:16]3[cH:17][cH:18][c:19]([Br:20])[cH:2...
CC(C)(C)OC(=O)N1CCNCC1.Clc1ccnc2ccc(Br)cc12
CC(C)(C)OC(=O)N1CCN(c2ccnc3ccc(Br)cc23)CC1
null
null
O.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
9f69c5c4a4ea31f8d76ec3987be7bd40b9cb34092e5d3f4fe2f7075ca0afa5f4
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(N3CCNCC3)ccnc2c1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[#7:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[c:6]:[c:5]1:[#7;a:4]:[c:3]:[c:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:12]2-[C:13]-[C:14]-[#7:9]-[C:10]-[C:11]-2):[c:7]:1:[c:8]
71.7
[{"value": 71.7, "product": "BrC=1C=C2C(=CC=NC2=CC1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
8
HOUR
A mixture of 243 mg 6-bromo-4-chloroquinoline, 373 mg t-butyl 1-piperazine carboxylate, 0.28 mL triethylamine and 10 mL dimethyl sulfoxide was stirred at 80° C. overnight. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated, washed twice with water and then with brine and dr...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1C[NH]CCN1.c1ccc2ncccc2c1
C1C[NH]CC[NH]1.c1ccc2ncccc2c1
C1C[NH]CC[NH]1.c1ccc2ncccc2c1
HCl
O.C(C)(=O)OCC
80
8
CC(C)(C)OC(=O)N1CCNCC1.Clc1ccnc2ccc(Br)cc12>O.C(C)(=O)OCC>CC(C)(C)OC(=O)N1CCN(c2ccnc3ccc(Br)cc23)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-81d64fbcd2ec4401aa24fe933c90a8e1
COC1CCNCC1.Clc1ccnc2ccc(Br)cc12>>COC1CCN(c2ccnc3ccc(Br)cc23)CC1
BrC=1C=C2C(=CC=NC2=CC1)Cl.Cl.COC1CCNCC1.C(C)N(CC)CC.CN(C=O)C>>COC1CCN(CC1)C1=CC=NC2=CC=C(C=C12)Br
[CH3:1][O:2][CH:3]1[CH2:4][CH2:5][NH:6][CH2:18][CH2:19]1.Cl[c:7]1[cH:8][cH:9][n:10][c:11]2[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]12>>[CH3:1][O:2][CH:3]1[CH2:4][CH2:5][N:6]([c:7]2[cH:8][cH:9][n:10][c:11]3[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]23)[CH2:18][CH2:19]1
COC1CCNCC1.Clc1ccnc2ccc(Br)cc12
COC1CCN(c2ccnc3ccc(Br)cc23)CC1
null
null
O.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
6ca896bdf5cf17e98a9402041cc62e117ebb3e6ff582ec413fbc5219ab9874c5
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(N3CCCCC3)ccnc2c1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[C:9]-[C:10]-[NH;D2;+0:11]-[C:12]-[C:13]>>[C:9]-[C:10]-[N;H0;D3;+0:11](-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8])-[C:12]-[C:13]
77.9
[{"value": 77.9, "product": "COC1CCN(CC1)C1=CC=NC2=CC=C(C=C12)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
130
CELSIUS
8
HOUR
A mixture of 500 mg 6-bromo-4-chloroquinoline, 330 mg 4-methoxypiperidine monohydrochloride, 0.57 mL triethylamine and 10 mL N,N-dimethylformamide was stirred at 130° C. for 8 hours. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated. The organic layer was washed with water...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CCNCC1.c1ccc2ncccc2c1
C1CC[NH]CC1.c1ccc2ncccc2c1
C1CC[NH]CC1.c1ccc2ncccc2c1
HCl
O.C(C)(=O)OCC
130
8
COC1CCNCC1.Clc1ccnc2ccc(Br)cc12>O.C(C)(=O)OCC>COC1CCN(c2ccnc3ccc(Br)cc23)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-89fd9da20ba146b4ac2f3d471bf591bc
CO[C@H]1CNC[C@@H]1OC.Clc1ccnc2ccc(Br)cc12>>CO[C@H]1CN(c2ccnc3ccc(Br)cc23)C[C@@H]1OC
BrC=1C=C2C(=CC=NC2=CC1)Cl.Cl.CO[C@H]1CNC[C@@H]1OC>>BrC=1C=C2C(=CC=NC2=CC1)N1C[C@@H]([C@H](C1)OC)OC
[CH3:1][O:2][C@H:3]1[CH2:4][NH:5][CH2:17][C@@H:18]1[O:19][CH3:20].Cl[c:6]1[cH:7][cH:8][n:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]12>>[CH3:1][O:2][C@H:3]1[CH2:4][N:5]([c:6]2[cH:7][cH:8][n:9][c:10]3[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]23)[CH2:17][C@@H:18]1[O:19][CH3:20]
CO[C@H]1CNC[C@@H]1OC.Clc1ccnc2ccc(Br)cc12
CO[C@H]1CN(c2ccnc3ccc(Br)cc23)C[C@@H]1OC
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
89f800d0b5c6eace023ec0f16ed65844f5dd409e156b3b4845e1db5de9a38872
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(N3CCCC3)ccnc2c1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[C:9]1-[C:10]-[C:11]-[C:12]-[NH;D2;+0:13]-1>>[c:6]:[c:5]1:[#7;a:4]:[c:3]:[c:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:13]2-[C:9]-[C:10]-[C:11]-[C:12]-2):[c:7]:1:[c:8]
35.7
[{"value": 35.7, "product": "BrC=1C=C2C(=CC=NC2=CC1)N1C[C@@H]([C@H](C1)OC)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
697 mg 6-bromo-4-chloroquinoline and 482 mg (3S,4S)-3,4-dimethoxytetrahydro-1H pyrrole monohydrochloride were reacted by the same method as in Production Example 82, to give 346 mg of the title compound as pale brown crystals. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CCNC1.c1ccc2ncccc2c1
C1CC[NH]C1.c1ccc2ncccc2c1
C1CC[NH]C1.c1ccc2ncccc2c1
HCl
null
null
null
CO[C@H]1CNC[C@@H]1OC.Clc1ccnc2ccc(Br)cc12>>CO[C@H]1CN(c2ccnc3ccc(Br)cc23)C[C@@H]1OC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-44a5b37683ee46fc947e367ce6e12229
CO[C@@H]1CCNC1.Clc1ccnc2ccc(Br)cc12>>CO[C@@H]1CCN(c2ccnc3ccc(Br)cc23)C1
BrC=1C=C2C(=CC=NC2=CC1)Cl.Cl.CO[C@H]1CNCC1>>BrC=1C=C2C(=CC=NC2=CC1)N1C[C@@H](CC1)OC
[CH3:1][O:2][C@@H:3]1[CH2:4][CH2:5][NH:6][CH2:18]1.Cl[c:7]1[cH:8][cH:9][n:10][c:11]2[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]12>>[CH3:1][O:2][C@@H:3]1[CH2:4][CH2:5][N:6]([c:7]2[cH:8][cH:9][n:10][c:11]3[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]23)[CH2:18]1
CO[C@@H]1CCNC1.Clc1ccnc2ccc(Br)cc12
CO[C@@H]1CCN(c2ccnc3ccc(Br)cc23)C1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
89f800d0b5c6eace023ec0f16ed65844f5dd409e156b3b4845e1db5de9a38872
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(N3CCCC3)ccnc2c1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[C:9]1-[C:10]-[C:11]-[C:12]-[NH;D2;+0:13]-1>>[c:6]:[c:5]1:[#7;a:4]:[c:3]:[c:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:13]2-[C:9]-[C:10]-[C:11]-[C:12]-2):[c:7]:1:[c:8]
44.8
[{"value": 44.8, "product": "BrC=1C=C2C(=CC=NC2=CC1)N1C[C@@H](CC1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
500 mg 6-bromo-4-chloroquinoline and 300 mg (3R)-3-methoxy pyrrolidine monohydrochloride were reacted by the same method as in Production Example 82, to give 284 mg of the title compound as a yellow oil. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CCNC1.c1ccc2ncccc2c1
C1CC[NH]C1.c1ccc2ncccc2c1
C1CC[NH]C1.c1ccc2ncccc2c1
HCl
null
null
null
CO[C@@H]1CCNC1.Clc1ccnc2ccc(Br)cc12>>CO[C@@H]1CCN(c2ccnc3ccc(Br)cc23)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2b980d3bc2484497869d7efaf50a8779
Clc1ccnc2ccc(Br)cc12.c1ccc(OC2CCNCC2)nc1>>Brc1ccc2nccc(N3CCC(Oc4ccccn4)CC3)c2c1
BrC=1C=C2C(=CC=NC2=CC1)Cl.Cl.Cl.N1CCC(CC1)OC1=NC=CC=C1>>BrC=1C=C2C(=CC=NC2=CC1)N1CCC(CC1)OC1=NC=CC=C1
Cl[c:9]1[cH:8][cH:7][n:6][c:5]2[cH:4][cH:3][c:2]([Br:1])[cH:24][c:23]21.[NH:10]1[CH2:11][CH2:12][CH:13]([O:14][c:15]2[cH:16][cH:17][cH:18][cH:19][n:20]2)[CH2:21][CH2:22]1>>[Br:1][c:2]1[cH:3][cH:4][c:5]2[n:6][cH:7][cH:8][c:9]([N:10]3[CH2:11][CH2:12][CH:13]([O:14][c:15]4[cH:16][cH:17][cH:18][cH:19][n:20]4)[CH2:21][CH2:22...
Clc1ccnc2ccc(Br)cc12.c1ccc(OC2CCNCC2)nc1
Brc1ccc2nccc(N3CCC(Oc4ccccn4)CC3)c2c1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
6ca896bdf5cf17e98a9402041cc62e117ebb3e6ff582ec413fbc5219ab9874c5
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc(OC2CCN(c3ccnc4ccccc34)CC2)nc1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[C:9]-[C:10]-[NH;D2;+0:11]-[C:12]-[C:13]>>[C:9]-[C:10]-[N;H0;D3;+0:11](-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8])-[C:12]-[C:13]
79.4
[{"value": 79.4, "product": "BrC=1C=C2C(=CC=NC2=CC1)N1CCC(CC1)OC1=NC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
500 mg 6-bromo-4-chloroquinoline and 540 mg 2-(4-piperidyloxy) pyridine dihydrochloride were reacted by the same method as in Production Example 82, to give 629 mg of the title compound as an orange oil. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
c1ccc2ncccc2c1.C1CCNCC1
c1ccc2ncccc2c1.C1CC[NH]CC1
c1ccc2ncccc2c1.C1CC[NH]CC1.c1ccncc1
HCl
null
null
null
Clc1ccnc2ccc(Br)cc12.c1ccc(OC2CCNCC2)nc1>>Brc1ccc2nccc(N3CCC(Oc4ccccn4)CC3)c2c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f7a48dd0422e4d15afe9cbf385fb152a
CCOC(=O)C1CCNCC1.Clc1ccnc2ccc(Br)cc12>>CCOC(=O)C1CCN(c2ccnc3ccc(Br)cc23)CC1
BrC=1C=C2C(=CC=NC2=CC1)Cl.N1CCC(CC1)C(=O)OCC>>BrC=1C=C2C(=CC=NC2=CC1)N1CCC(CC1)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]1[CH2:7][CH2:8][NH:9][CH2:21][CH2:22]1.Cl[c:10]1[cH:11][cH:12][n:13][c:14]2[cH:15][cH:16][c:17]([Br:18])[cH:19][c:20]12>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]1[CH2:7][CH2:8][N:9]([c:10]2[cH:11][cH:12][n:13][c:14]3[cH:15][cH:16][c:17]([Br:18])[cH:19][c:20]23)[CH2:21][CH2:22]1
CCOC(=O)C1CCNCC1.Clc1ccnc2ccc(Br)cc12
CCOC(=O)C1CCN(c2ccnc3ccc(Br)cc23)CC1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
6ca896bdf5cf17e98a9402041cc62e117ebb3e6ff582ec413fbc5219ab9874c5
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(N3CCCCC3)ccnc2c1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[C:9]-[C:10]-[NH;D2;+0:11]-[C:12]-[C:13]>>[C:9]-[C:10]-[N;H0;D3;+0:11](-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8])-[C:12]-[C:13]
64.1
[{"value": 64.1, "product": "BrC=1C=C2C(=CC=NC2=CC1)N1CCC(CC1)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
500 mg 6-bromo-4-chloroquinoline and 340 mg ethyl 4-piperidine carboxylate were reacted by the same method as in Production Example 74, to give 480 mg of the title compound as a yellow oil. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CCNCC1.c1ccc2ncccc2c1
C1CC[NH]CC1.c1ccc2ncccc2c1
C1CC[NH]CC1.c1ccc2ncccc2c1
HCl
null
null
null
CCOC(=O)C1CCNCC1.Clc1ccnc2ccc(Br)cc12>>CCOC(=O)C1CCN(c2ccnc3ccc(Br)cc23)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4b79f5dff96f4fe7a29b5ace3d4445d4
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1cccs1.Clc1ncnc2ccc(Br)cc12>>Brc1ccc2ncnc(-c3cccs3)c2c1
BrC=1C=C2C(=NC=NC2=CC1)Cl.C(CCC)[Sn](C=1SC=CC1)(CCCC)CCCC>>BrC=1C=C2C(=NC=NC2=CC1)C=1SC=CC1
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c:10]1[cH:11][cH:12][cH:13][s:14]1.Cl[c:9]1[n:8][cH:7][n:6][c:5]2[cH:4][cH:3][c:2]([Br:1])[cH:16][c:15]21>>[Br:1][c:2]1[cH:3][cH:4][c:5]2[n:6][cH:7][n:8][c:9](-[c:10]3[cH:11][cH:12][cH:13][s:14]3)[c:15]2[cH:16]1
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1cccs1.Clc1ncnc2ccc(Br)cc12
Brc1ccc2ncnc(-c3cccs3)c2c1
null
null
C1(=CC=CC=C1)C
C-C Coupling
Stille reaction_aryl
9d6933a964770fa23bac63577249a9b6209b9d6653ec0f7df7a6a7fbd8151548
db27eeefac0475c6d74fa10b3167e95a61caaae74e8bbafd45892452c0c3d4d6
c1csc(-c2ncnc3ccccc23)c1
C-C-C-[CH2]-[Sn](-[CH2]-C-C-C)(-[CH2]-C-C-C)-[c;H0;D3;+0:1]1:[#16;a:2]:[c:3]:[c:4]:[c:5]:1.Cl-[c;H0;D3;+0:6]1:[#7;a:7]:[c:8]:[#7;a:9]:[c:10](:[c:11]):[c:12]:1:[c:13]>>[c:13]:[c:12]1:[c:10](:[c:11]):[#7;a:9]:[c:8]:[#7;a:7]:[c;H0;D3;+0:6]:1-[c;H0;D3;+0:1]1:[#16;a:2]:[c:3]:[c:4]:[c:5]:1
null
[]
80
CELSIUS
24
HOUR
0.6 g 6-bromo-4-chloroquinazoline was dissolved in 18 mL toluene, and 0.82 mL tri-n-butyl(2-thienyl)stannane and 0.14 g tetrakis (triphenylphosphine)palladium (0) were added thereto and stirred at 80° C. for 24 hours under nitrogen atmosphere. After the solvent was evaporated, the residue was purified by silica gel chr...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tin
null
c1ccsc1.c1ccc2ncncc2c1
c1ccc2ncncc2c1.c1ccsc1
c1ccc2ncncc2c1.c1ccsc1
HCl.Sn
C1(=CC=CC=C1)C
80
24
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1cccs1.Clc1ncnc2ccc(Br)cc12>C1(=CC=CC=C1)C>Brc1ccc2ncnc(-c3cccs3)c2c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3c5a26d55dd54e2e9666e23a47ffb5d3
Clc1ncnc2ccc(Br)cc12.FC(F)(F)c1cccc(N2CCNCC2)c1>>FC(F)(F)c1cccc(N2CCN(c3ncnc4ccc(Br)cc34)CC2)c1
BrC=1C=C2C(=NC=NC2=CC1)Cl.FC(C=1C=C(C=CC1)N1CCNCC1)(F)F.C(C)N(CC)CC>>BrC=1C=C2C(=NC=NC2=CC1)N1CCN(CC1)C1=CC(=CC=C1)C(F)(F)F
Cl[c:14]1[n:15][cH:16][n:17][c:18]2[cH:19][cH:20][c:21]([Br:22])[cH:23][c:24]12.[F:1][C:2]([F:3])([F:4])[c:5]1[cH:6][cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][NH:13][CH2:25][CH2:26]2)[cH:27]1>>[F:1][C:2]([F:3])([F:4])[c:5]1[cH:6][cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][N:13]([c:14]3[n:15][cH:16][n:17][c:18]4[cH:19][cH:...
Clc1ncnc2ccc(Br)cc12.FC(F)(F)c1cccc(N2CCNCC2)c1
FC(F)(F)c1cccc(N2CCN(c3ncnc4ccc(Br)cc34)CC2)c1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
bf3493eee827560da1b96eed7238401d257cea1a4f36eecd786eab0e1b0d6849
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc(N2CCN(c3ncnc4ccccc34)CC2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](:[c:6]):[c:7]:1:[c:8].[#7:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[c:6]:[c:5]1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:12]2-[C:11]-[C:10]-[#7:9]-[C:14]-[C:13]-2):[c:7]:1:[c:8]
66.8
[{"value": 66.8, "product": "BrC=1C=C2C(=NC=NC2=CC1)N1CCN(CC1)C1=CC(=CC=C1)C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
A mixture of 300 mg 6-bromo-4-chloroquinazoline, 350 mg 1-[3-(trifluoromethyl)phenyl]piperazine, 0.18 mL triethylamine and 5 mL N,N-dimethylformamide was stirred at room temperature for 4 hours. After the solvent was evaporated, the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
c1ccc2ncncc2c1.C1C[NH]CCN1
C1C[NH]CC[NH]1.c1ccc2ncncc2c1
c1ccccc1.C1C[NH]CC[NH]1.c1ccc2ncncc2c1
HCl
CN(C=O)C
null
4
Clc1ncnc2ccc(Br)cc12.FC(F)(F)c1cccc(N2CCNCC2)c1>CN(C=O)C>FC(F)(F)c1cccc(N2CCN(c3ncnc4ccc(Br)cc34)CC2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e03a8a5d6a4d424ba1fe1ef24c7a44ef
N#CCc1ccc(F)cc1.O=[N+]([O-])c1ccc(Br)cc1>>Fc1ccc(-c2onc3ccc(Br)cc23)cc1
O.BrC1=CC=C(C=C1)[N+](=O)[O-].FC1=CC=C(C=C1)CC#N.[OH-].[Na+]>>BrC1=CC=2C(=NOC2C2=CC=C(C=C2)F)C=C1
N#C[CH2:6][c:5]1[cH:4][cH:3][c:2]([F:1])[cH:17][cH:16]1.O=[N+:8]([O-:7])[c:9]1[cH:10][cH:11][c:12]([Br:13])[cH:14][cH:15]1>>[F:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[o:7][n:8][c:9]3[cH:10][cH:11][c:12]([Br:13])[cH:14][c:15]23)[cH:16][cH:17]1
N#CCc1ccc(F)cc1.O=[N+]([O-])c1ccc(Br)cc1
Fc1ccc(-c2onc3ccc(Br)cc23)cc1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
0f22d84b2a4c2a0e4579a9b5d1adb0e1a3a85c6a163e0b5818a361e01201e52a
b0095d38e0fbba4b05f88363393446922ef1c66394cfc608f7c1cd4fc808583a
c1ccc(-c2onc3ccccc23)cc1
N#C-[CH2;D2;+0:1]-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5]:[c:6].O=[N+;H0;D3:7](-[O-;H0;D1:8])-[c:9](:[c:10]):[cH;D2;+0:11]:[c:12]:[c:13]>>[c:10]:[c:9]1:[n;H0;D2;+0:7]:[o;H0;D2;+0:8]:[c;H0;D3;+0:1](-[c;H0;D3;+0:2](:[c:3]:[c:4]):[c:5]:[c:6]):[c;H0;D3;+0:11]:1:[c:12]:[c:13]
null
[]
null
null
null
null
13 g 1-bromo-4-nitrobenzene, 7.68 mL 2-(4-fluorophenyl)acetonitrile and 3.9 g sodium hydroxide were stirred in 130 mL ethanol at 40° C. for 24 hours. After the reaction solution was left and cooled, water was added thereto and the reaction solution was extracted with ethylacetate. The organic solvent was washed with br...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Nitro group
null
c1ccccc1
c1ccc2nocc2c1
c1ccccc1.c1ccc2nocc2c1
HO-
C(C)O
null
null
N#CCc1ccc(F)cc1.O=[N+]([O-])c1ccc(Br)cc1>C(C)O>Fc1ccc(-c2onc3ccc(Br)cc23)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4041fef8b4e54995b5089ae87eb6ab96
COC(=O)c1ccc(-c2ccn(C(c3ccccc3)(c3ccccc3)c3ccccc3)n2)s1.O=C1CCC(=O)N1I>>COC(=O)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2I)s1
C(C1=CC=CC=C1)(C1=CC=CC=C1)(C1=CC=CC=C1)N1N=C(C=C1)C1=CC=C(S1)C(=O)OC.IN1C(CCC1=O)=O.S(=S)(=O)([O-])[O-].[Na+].[Na+].C([O-])(O)=O.[Na+].IN1C(CCC1=O)=O>>IC=1C(=NN(C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=C(S1)C(=O)OC
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8](-[c:9]2[n:10][n:11]([C:12]([c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)([c:19]3[cH:20][cH:21][cH:22][cH:23][cH:24]3)[c:25]3[cH:26][cH:27][cH:28][cH:29][cH:30]3)[cH:31][cH:32]2)[s:34]1.O=C1CCC(=O)N1[I:33]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8](-[c:9]2[n:10][n:1...
COC(=O)c1ccc(-c2ccn(C(c3ccccc3)(c3ccccc3)c3ccccc3)n2)s1.O=C1CCC(=O)N1I
COC(=O)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2I)s1
null
null
CN(C=O)C
Functional Group Interconversion
OtherReaction
13d4025b7e4d89e18a4bdf4324e272b69308705ca7d8d86b51c72ac440b14757
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccc(C(c2ccccc2)(c2ccccc2)n2ccc(-c3cccs3)n2)cc1
O=C1-C-C-C(=O)-N-1-[I;H0;D1;+0:1].[#16;a:2]:[c:3]-[c:4]1:[#7;a:5]:[#7;a:6](-[C:7]):[c:8]:[cH;D2;+0:9]:1>>[#16;a:2]:[c:3]-[c:4]1:[#7;a:5]:[#7;a:6](-[C:7]):[c:8]:[c;H0;D3;+0:9]:1-[I;H0;D1;+0:1]
95.7
[{"value": 95.7, "product": "IC=1C(=NN(C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=C(S1)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
24
HOUR
20 g methyl 5-(1-trityl-1H-3-pyrazolyl)-2-thiophene carboxylate and 10.6 g N-iodosuccinimide were stirred in 200 mL N,N-dimethylformamide at 80° C. for 24 hours. Additional N-iodosuccinimide, 10.6 g, was added thereto and stirred at 80° C. for 24 hours, and then an aqueous solution of sodium thiosulfate and an aqueous ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1ccn[nH]1.C1CCNC1
c1c[nH]nc1
c1ccsc1.c1c[nH]nc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
CN(C=O)C
80
24
COC(=O)c1ccc(-c2ccn(C(c3ccccc3)(c3ccccc3)c3ccccc3)n2)s1.O=C1CCC(=O)N1I>CN(C=O)C>COC(=O)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2I)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d4c5a74becb748159582e59b4d9a4a5e
CC(=O)c1ccc(O)cc1.C[Si](C)(C)CCOCCl>>CC(=O)c1ccc(OCOCC[Si](C)(C)C)cc1
C[Si](CCOCCl)(C)C.CC(=O)C=1C=CC(=CC1)O.C(C)(C)N(CC)C(C)C>>C[Si](CCOCOC1=CC=C(C=C1)C(C)=O)(C)C
[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]([OH:8])[cH:17][cH:18]1.Cl[CH2:9][O:10][CH2:11][CH2:12][Si:13]([CH3:14])([CH3:15])[CH3:16]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]([O:8][CH2:9][O:10][CH2:11][CH2:12][Si:13]([CH3:14])([CH3:15])[CH3:16])[cH:17][cH:18]1
CC(=O)c1ccc(O)cc1.C[Si](C)(C)CCOCCl
CC(=O)c1ccc(OCOCC[Si](C)(C)C)cc1
null
null
ClCCl
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
6e90ffbf0683e1a3ee55c5e3ea453aefc5ddd369c0150ed0150f9546d7e47f4f
efd670663709b79afcad1306da9f69b33a0147cfa3639ca4c0b54b35ef4b1852
c1ccccc1
Cl-[CH2;D2;+0:1]-[#8:2]-[C:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[#8:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
null
[]
null
null
4
HOUR
While 30 mL solution of 2.72 g 4-hydroxyacetophenone and 5.2 mL diisopropyl ethylamine in dichloromethane was stirred under ice-cooling in a stream of nitrogen, 4.2 mL 2-(trimethylsilyl)ethoxymethyl chloride was added thereto. Then, the reaction solution was stirred at room temperature for 4 hours. The reaction solutio...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Aromatic alcohol
Ether.Ether
null
null
c1ccccc1
HCl
ClCCl
null
4
CC(=O)c1ccc(O)cc1.C[Si](C)(C)CCOCCl>ClCCl>CC(=O)c1ccc(OCOCC[Si](C)(C)C)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1b320b4caf48445d87272a3586e3dd76
Nc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1>>CN(C)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1
C(C)(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+].BrC=1C(=NN(C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=C(C=C1)N.C(=O)N.C([O-])(O)=O.[Na+]>>BrC=1C(=NN(C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=C(C=C1)N(C)C
[NH2:2][c:4]1[cH:5][cH:6][c:7](-[c:8]2[n:9][n:10]([C:11]([c:12]3[cH:13][cH:14][cH:15][cH:16][cH:17]3)([c:18]3[cH:19][cH:20][cH:21][cH:22][cH:23]3)[c:24]3[cH:25][cH:26][cH:27][cH:28][cH:29]3)[cH:30][c:31]2[Br:32])[cH:33][cH:34]1>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7](-[c:8]2[n:9][n:10]([C:11]([c:12]3[cH:13][cH:14...
Nc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1
CN(C)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1
null
null
O.ClCCCl.C(C)(=O)OCC
Miscellaneous
OtherReaction
0295391ed0de2e86c7e882f3199152884d99da63bc1b927b39500202e1a00977
98c3809a8b4046b29490f9afb6277ec8718e0550ab1278bc09b7f0dc821fa6fe
c1ccc(-c2ccn(C(c3ccccc3)(c3ccccc3)c3ccccc3)n2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]>>[C;D1;H3:5]-[N;H0;D3;+0:1](-[C;D1;H3:6])-[c:2](:[c:3]):[c:4]
null
[]
null
null
3
DAY
2.54 g sodium triacetoxy borohydride was added little by little at room temperature to a mixture of 1.44 g 4-(4-bromo-1-trityl-1H-pyrazol-3-yl)phenylamine (compound in Production Example 152), 0.61 mL of 37% formamide and 40 mL 1,2-dichloroethane, and the mixture was stirred for 3 days. Ethyl acetate and an aqueous sat...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Tertiary amine
null
null
c1ccccc1.c1c[nH]nc1.c1ccccc1.c1ccccc1.c1ccccc1
Other
O.ClCCCl.C(C)(=O)OCC
null
72
Nc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1>O.ClCCCl.C(C)(=O)OCC>CN(C)c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9de829fad7074c198d36aaffabd3acbe
BrCCOCCBr.Nc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1>>Brc1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(N2CCOCC2)cc1
BrC=1C(=NN(C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=C(C=C1)N.BrCCOCCBr.[I-].[Na+].C([O-])([O-])=O.[K+].[K+]>>BrC=1C(=NN(C1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=C(C=C1)N1CCOCC1
Br[CH2:31][CH2:32][O:33][CH2:34][CH2:35]Br.[Br:1][c:2]1[cH:3][n:4]([C:5]([c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)([c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)[n:24][c:25]1-[c:26]1[cH:27][cH:28][c:29]([NH2:30])[cH:36][cH:37]1>>[Br:1][c:2]1[cH:3][n:4]([C:5]([c:6]2[cH:7][cH:8][c...
BrCCOCCBr.Nc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1
Brc1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(N2CCOCC2)cc1
null
null
O.CN(C=O)C.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
96e983e5a21a49df63baecef913e7d3b8dacd6365c270725738379ba775c02bb
631870b1ab33be0edc94bc9ae10321f1c5ede4dd4db77035c9d3979e4a2118fb
c1ccc(C(c2ccccc2)(c2ccccc2)n2ccc(-c3ccc(N4CCOCC4)cc3)n2)cc1
Br-[CH2;D2;+0:1]-[C:2]-[#8:3]-[C:4]-[CH2;D2;+0:5]-Br.[NH2;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[c:8]:[c:7](-[N;H0;D3;+0:6]1-[CH2;D2;+0:1]-[C:2]-[#8:3]-[C:4]-[CH2;D2;+0:5]-1):[c:9]
null
[]
80
CELSIUS
3
DAY
A mixture of 2.4 g 4-(4-bromo-1-trityl-1H-pyrazol-3-yl)phenylamine (compound in Production Example 152), 0.7 mL 2-bromoethyl ether, 80 mg sodium iodide, 1.52 g potassium carbonate and 50 mL N,N-dimethylformamide was stirred at 80° C. for 3 days. Ethyl acetate and water were added to the reaction solution, then water wa...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Primary amine
Tertiary amine
null
C1COCC[NH]1
c1cn[nH]c1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1.C1COCC[NH]1
HBr
O.CN(C=O)C.C(C)(=O)OCC
80
72
BrCCOCCBr.Nc1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2Br)cc1>O.CN(C=O)C.C(C)(=O)OCC>Brc1cn(C(c2ccccc2)(c2ccccc2)c2ccccc2)nc1-c1ccc(N2CCOCC2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7e06764fbfd84dcfb07798a6103e3bba
C=[C](OCC)[Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.Cc1ccc(Br)c(F)c1>>CC(=O)c1ccc(C)cc1F
BrC1=C(C=C(C=C1)C)F.C(CCC)[Sn](C(=C)OCC)(CCCC)CCCC>>FC1=C(C=CC(=C1)C)C(C)=O
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[C:2](=[CH2:1])[O:3]CC.Br[c:4]1[cH:5][cH:6][c:7]([CH3:8])[cH:9][c:10]1[F:11]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]([CH3:8])[cH:9][c:10]1[F:11]
C=[C](OCC)[Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.Cc1ccc(Br)c(F)c1
CC(=O)c1ccc(C)cc1F
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
[F-].[K+].C1(=CC=CC=C1)C.C(C)(=O)OCC
Acylation
OtherReaction
e81a9e4f1410d41358aeb55fc26a37a1b785aea938455868d964ef705a085ee2
63004495c3d76884d1ef7552ef244f48fc0c4b379316352f7c7b6b3ce0e8b2c8
c1ccccc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[F;D1;H0:5]):[c:6].C-C-C-[CH2]-[Sn](-[CH2]-C-C-C)(-[CH2]-C-C-C)-[C;H0;D3;+0:7](=[CH2;D1;+0:8])-[O;H0;D2;+0:9]-C-C>>[CH3;D1;+0:8]-[C;H0;D3;+0:7](=[O;H0;D1;+0:9])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[F;D1;H0:5]):[c:6]
114.5
[{"value": 114.5, "product": "FC1=C(C=CC(=C1)C)C(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
54 mL solution of 5.0 g 1-bromo-2-fluoro-4-methylbenzene, 10 g tributyl(1-ethoxyvinyl)tin and 1.53 g tetrakis (triphenylphosphine) palladium in toluene was heated at 120° C. for 2 hours. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate, 10% aqueous potassium fluoride solution was a...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ether.Vinyl.Tin
Ketone
c1ccccc1
c1ccccc1
c1ccccc1
HBr.Sn
[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.[F-].[K+].C1(=CC=CC=C1)C.C(C)(=O)OCC
null
0.5
C=[C](OCC)[Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.Cc1ccc(Br)c(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.[F-].[K+].C1(=CC=CC=C1)C.C(C)(=O)OCC>CC(=O)c1ccc(C)cc1F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f1c2816f2f184ef9a353812df19c64f4
CC(=O)c1ccc(F)cc1F.COCCO>>COCCOc1cc(F)ccc1C(C)=O
O.COCCO.[H-].[Na+].FC1=C(C=CC(=C1)F)C(C)=O>>FC1=CC(=C(C=C1)C(C)=O)OCCOC
F[c:6]1[cH:7][c:8]([F:9])[cH:10][cH:11][c:12]1[C:13]([CH3:14])=[O:15].[CH3:1][O:2][CH2:3][CH2:4][OH:5]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][c:6]1[cH:7][c:8]([F:9])[cH:10][cH:11][c:12]1[C:13]([CH3:14])=[O:15]
CC(=O)c1ccc(F)cc1F.COCCO
COCCOc1cc(F)ccc1C(C)=O
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
4821d6d7238522ee9ef4538c00647e855becf4de3d9c939c0cec2b01c1e5e915
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5](-[C;D1;H3:6])=[O;D1;H0:7]):[c:8].[C:9]-[C:10]-[OH;D1;+0:11]>>[C:9]-[C:10]-[O;H0;D2;+0:11]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5](-[C;D1;H3:6])=[O;D1;H0:7]):[c:8]
69.6
[{"value": 69.6, "product": "FC1=CC(=C(C=C1)C(C)=O)OCCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution of 1.75 g 2-methoxy ethanol in tetrahydrofuran (23 mL) was added dropwise to a suspension of 0.84 g of 60% sodium hydride in tetrahydrofuran (21 mL), and subsequently a solution of 3.0 g 2′,4′-difluoroacetophenone in tetrahydrofuran (19 mL) was added dropwise thereto. The temperature of the mixture was incre...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1ccccc1
c1ccccc1
c1ccccc1
HF
O1CCCC1
null
24
CC(=O)c1ccc(F)cc1F.COCCO>O1CCCC1>COCCOc1cc(F)ccc1C(C)=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2159859012fe4ea19678cdf3cfd8ed9c
C1CCCC1.CC(=O)c1ccc(O)cc1F>>CC(=O)c1ccc(OC2CCCC2)cc1F
[Br-].C1CCCC1.OC1=CC(=C(C=C1)C(C)=O)F.[Br-].C1CCCC1.C([O-])([O-])=O.[Cs+].[Cs+]>>C1(CCCC1)OC1=CC(=C(C=C1)C(C)=O)F
[CH2:9]1[CH2:10][CH2:11][CH2:12][CH2:13]1.[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]([OH:8])[cH:14][c:15]1[F:16]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]([O:8][CH:9]2[CH2:10][CH2:11][CH2:12][CH2:13]2)[cH:14][c:15]1[F:16]
C1CCCC1.CC(=O)c1ccc(O)cc1F
CC(=O)c1ccc(OC2CCCC2)cc1F
null
null
C(C)#N.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
1b0b141bf6b317fb3f4853d99c0e21f208620be70a498da9a42860eb95c70530
0f0966e3597a58033417ecee71659f4d0c082f95d46b1e52c95541e6e4a59086
c1ccc(OC2CCCC2)cc1
[C:1]1-[C:2]-[C:3]-[C:4]-[CH2;D2;+0:5]-1.[OH;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[c:8]:[c:7](-[O;H0;D2;+0:6]-[CH;D3;+0:5]1-[C:1]-[C:2]-[C:3]-[C:4]-1):[c:9]
null
[]
70
CELSIUS
null
null
A suspension of 2.5 g 4′-hydroxy-2′-fluoroacetophenone, 2.0 mL cyclopentane bromide and 7.9 g cesium carbonate in acetonitrile (35 mL) was heated for 1 hour under reflux and then heated at 70° C. for 15 hours. Further, 1.0 mL cyclopentane bromide was added thereto, and the mixture was heated for 3 hours under reflux. T...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol
Ether
C1CCCC1
C1CCCC1
c1ccccc1.C1CCCC1
null
C(C)#N.C(C)(=O)OCC
70
null
C1CCCC1.CC(=O)c1ccc(O)cc1F>C(C)#N.C(C)(=O)OCC>CC(=O)c1ccc(OC2CCCC2)cc1F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4e23a5fb633e499fab4435e476f56b52
CC(C)(C)OC(=O)N1CCC(C=O)CC1.CSc1ccc(Br)cc1>>CSc1ccc(C(O)C2CCN(C(=O)OC(C)(C)C)CC2)cc1
C(CCC)[Li].[Cl-].[NH4+].C(=O)C1CCN(CC1)C(=O)OC(C)(C)C.BrC1=CC=C(C=C1)SC>>OC(C1CCN(CC1)C(=O)OC(C)(C)C)C1=CC=C(C=C1)SC
[CH:7](=[O:8])[CH:9]1[CH2:10][CH2:11][N:12]([C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[CH2:20][CH2:21]1.Br[c:6]1[cH:5][cH:4][c:3]([S:2][CH3:1])[cH:23][cH:22]1>>[CH3:1][S:2][c:3]1[cH:4][cH:5][c:6]([CH:7]([OH:8])[CH:9]2[CH2:10][CH2:11][N:12]([C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[CH2:20][C...
CC(C)(C)OC(=O)N1CCC(C=O)CC1.CSc1ccc(Br)cc1
CSc1ccc(C(O)C2CCN(C(=O)OC(C)(C)C)CC2)cc1
null
null
O1CCCC1.CCCCCC.O
C-C Coupling
Grignard_alcohol
0c8bc0f755f4d9a2cfce93ae43a9a9a531fa8ad86ff120aed0a18ba03c84e4d7
1c0bd0afc1d5e370e3c8193faf738f03752295e40fa0eb99c756011e9a4be26b
c1ccc(CC2CCNCC2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[C:6]-[C:7](-[CH;D2;+0:8]=[O;H0;D1;+0:9])-[C:10]>>[C:6]-[C:7](-[CH;D3;+0:8](-[OH;D1;+0:9])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5])-[C:10]
23.8
[{"value": 23.8, "product": "OC(C1CCN(CC1)C(=O)OC(C)(C)C)C1=CC=C(C=C1)SC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
380 mg of 1-bromo-4-methylsulfanyl benzene was dissolved in 10 mL anhydrous tetrahydrofuran, and 1.24 mL solution of 1.59 M n-butyl lithium in hexane was added dropwise thereto at −70° C. After the mixture was stirred for 1 hour, 3 mL solution of 400 mg t-butyl 4-formyl-piperidine-1-carboxylate in anhydrous tetrahydrof...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aldehyde
Secondary alcohol
c1ccccc1
c1ccccc1
c1ccccc1.C1CC[NH]CC1
Br-
O1CCCC1.CCCCCC.O
0
1
CC(C)(C)OC(=O)N1CCC(C=O)CC1.CSc1ccc(Br)cc1>O1CCCC1.CCCCCC.O>CSc1ccc(C(O)C2CCN(C(=O)OC(C)(C)C)CC2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d734a28c973d447fb5fa90364bc5b07d
Clc1cccnc1Cl.NCCO>>OCCNc1ncccc1Cl
ClC1=NC=CC=C1Cl.NCCO.C([O-])(O)=O.[Na+]>>ClC=1C(=NC=CC1)NCCO
Cl[c:5]1[n:6][cH:7][cH:8][cH:9][c:10]1[Cl:11].[OH:1][CH2:2][CH2:3][NH2:4]>>[OH:1][CH2:2][CH2:3][NH:4][c:5]1[n:6][cH:7][cH:8][cH:9][c:10]1[Cl:11]
Clc1cccnc1Cl.NCCO
OCCNc1ncccc1Cl
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
c026a7bf7aba66b20cf21a13c528689aaaa1c05901524d62b36ca0c3b0572cef
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccncc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[Cl;D1;H0:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[Cl;D1;H0:5]):[c:6]
null
[]
null
null
null
null
After 11.46 g of 2,3-dichloropyridine and 9.8 mL 2-aminoethanol were heated at 100° C. for 24 hours, an aqueous saturated sodium bicarbonate solution was added thereto, and the reaction mixture was extracted with ethyl acetate. The extract was washed with brine, the organic layer was dried over anhydrous sodium sulfate...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccncc1
c1ccncc1
c1ccncc1
HCl
null
null
null
Clc1cccnc1Cl.NCCO>>OCCNc1ncccc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-015fb88594894c9e9b8be65f3fc280b6
O=C1CCC(=O)N1Br.OCCNc1ncccc1Cl>>OCCNc1ncc(Br)cc1Cl
ClC=1C(=NC=CC1)NCCO.BrN1C(CCC1=O)=O>>BrC=1C=C(C(=NC1)NCCO)Cl
O=C1CCC(=O)N1[Br:9].[OH:1][CH2:2][CH2:3][NH:4][c:5]1[n:6][cH:7][cH:8][cH:10][c:11]1[Cl:12]>>[OH:1][CH2:2][CH2:3][NH:4][c:5]1[n:6][cH:7][c:8]([Br:9])[cH:10][c:11]1[Cl:12]
O=C1CCC(=O)N1Br.OCCNc1ncccc1Cl
OCCNc1ncc(Br)cc1Cl
null
null
ClCCl.C(C)(=O)OCC
Functional Group Interconversion
Bromination
0c4eeb30070e87daf86c6fe6be8db4805f592c36398c82b1c29b987bb0b889d8
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccncc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[#7;a:2]1:[c:3]:[c:4]:[c:5]:[cH;D2;+0:6]:[c:7]:1>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:6]1:[c:5]:[c:4]:[c:3]:[#7;a:2]:[c:7]:1
103.6
[{"value": 103.6, "product": "BrC=1C=C(C(=NC1)NCCO)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
2.1 g of 2-(3-chloro-2-pyridinylamino)ethanol was dissolved in 25 mL dichloromethane, and 2.3 g N-bromosuccinimide was added little by little thereto at 0° C. and stirred for 1.5 hours. The reaction mixture was diluted with ethyl acetate and then washed with an aqueous saturated sodium bicarbonate and brine, the organi...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
C1CCNC1.c1ccncc1
c1ccncc1
c1ccncc1
HO-
ClCCl.C(C)(=O)OCC
null
1.5
O=C1CCC(=O)N1Br.OCCNc1ncccc1Cl>ClCCl.C(C)(=O)OCC>OCCNc1ncc(Br)cc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-841344a4b5f34e848713fd145538d083
ClC1=CC(Br)=CN2CCN=C12>>Clc1cc(Br)cn2ccnc12
BrC=1C=C(C=2N(C1)CCN2)Cl>>BrC=1C=C(C=2N(C1)C=CN2)Cl
[Cl:1][C:2]1=[CH:3][C:4]([Br:5])=[CH:6][N:7]2[CH2:8][CH2:9][N:10]=[C:11]12>>[Cl:1][c:2]1[cH:3][c:4]([Br:5])[cH:6][n:7]2[cH:8][cH:9][n:10][c:11]12
ClC1=CC(Br)=CN2CCN=C12
Clc1cc(Br)cn2ccnc12
null
[O-2].[O-2].[Mn+4]
CC(=O)C
Aromatic Heterocycle Formation
OtherReaction
f78e386d593b75391a5171d414f8e09c792e7ccc66325ae4c56fec3ba0d5884b
2c84cf48ded06568363103656ecd004a95adf46ead3e1488fc2053dc37ca8452
c1ccn2ccnc2c1
[Br;D1;H0:1]-[C;H0;D3;+0:2]1=[CH;D2;+0:3]-[N;H0;D3;+0:4]2-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[N;H0;D2;+0:7]=[C;H0;D3;+0:8]-2-[C;H0;D3;+0:9](-[Cl;D1;H0:10])=[CH;D2;+0:11]-1>>[Br;D1;H0:1]-[c;H0;D3;+0:2]1:[cH;D2;+0:11]:[c;H0;D3;+0:9](-[Cl;D1;H0:10]):[c;H0;D3;+0:8]2:[n;H0;D2;+0:7]:[cH;D2;+0:6]:[cH;D2;+0:5]:[n;H0;D3;+0:4]:2:[cH;D2...
61.6
[{"value": 61.6, "product": "BrC=1C=C(C=2N(C1)C=CN2)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2.08 g of 6-bromo-8-chloro-2,3-dihydroimidazo[1,2-a]pyridine was dissolved in 36 mL acetone, and together with 9.1 g of manganese dioxide, the mixture was heated for 9 hours under reflux. The reaction solution was cooled to room temperature, filtered through Celite and washed with ethyl acetate. The solvent was removed...
10.6084/m9.figshare.5104873.v1
null
Enamine.Alkenyl halide.Alkenyl halide
Aromatic halide.Aromatic halide
C1=CC2=NCCN2C=C1
c1ccn2ccnc2c1
c1ccn2ccnc2c1
null
[O-2].[O-2].[Mn+4].CC(=O)C
null
null
ClC1=CC(Br)=CN2CCN=C12>[O-2].[O-2].[Mn+4].CC(=O)C>Clc1cc(Br)cn2ccnc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7826fd182752414c9f1a1263d827f13b
Brc1ccc(Br)nc1.COC(CN)OC>>COC(CNc1ccc(Br)cn1)OC
BrC1=NC=C(C=C1)Br.COC(CN)OC.C([O-])(O)=O.[Na+]>>BrC=1C=CC(=NC1)NCC(OC)OC
Br[c:6]1[cH:7][cH:8][c:9]([Br:10])[cH:11][n:12]1.[CH3:1][O:2][CH:3]([CH2:4][NH2:5])[O:13][CH3:14]>>[CH3:1][O:2][CH:3]([CH2:4][NH:5][c:6]1[cH:7][cH:8][c:9]([Br:10])[cH:11][n:12]1)[O:13][CH3:14]
Brc1ccc(Br)nc1.COC(CN)OC
COC(CNc1ccc(Br)cn1)OC
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
c026a7bf7aba66b20cf21a13c528689aaaa1c05901524d62b36ca0c3b0572cef
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccncc1
Br-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
null
null
After 50 g of 2,5-dibromopyridine and 50 mL aminoacetaldehyde dimethyl acetal were heated at 130° C. for 8 hours, an aqueous saturated sodium bicarbonate solution was added thereto, and the reaction mixture was extracted with ethyl acetate. The extract was washed with brine, the organic layer was dried over anhydrous s...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccncc1
c1ccncc1
c1ccncc1
HBr
null
null
null
Brc1ccc(Br)nc1.COC(CN)OC>>COC(CNc1ccc(Br)cn1)OC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0dbdc9783d4d489ab198e2f789e8084b
Cc1ccc(S(=O)(=O)Cl)cc1.N#CC(O)CNc1ccc(Br)cn1>>Cc1ccc(S(=O)(=O)OC(C#N)CNc2ccc(Br)cn2)cc1
C([O-])(O)=O.[Na+].C(C)(C)N(CC)C(C)C.C1(=CC=C(C=C1)S(=O)(=O)Cl)C.BrC=1C=CC(=NC1)NCC(C#N)O>>C1(=CC=C(C=C1)S(=O)(=O)OC(CNC1=NC=C(C=C1)Br)C#N)C
Cl[S:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:23][cH:22]1)(=[O:7])=[O:8].[OH:9][CH:10]([C:11]#[N:12])[CH2:13][NH:14][c:15]1[cH:16][cH:17][c:18]([Br:19])[cH:20][n:21]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[O:9][CH:10]([C:11]#[N:12])[CH2:13][NH:14][c:15]2[cH:16][cH:17][c:18]([Br:19])[cH:20][n:21]2)[cH:22][c...
Cc1ccc(S(=O)(=O)Cl)cc1.N#CC(O)CNc1ccc(Br)cn1
Cc1ccc(S(=O)(=O)OC(C#N)CNc2ccc(Br)cn2)cc1
null
null
ClCCl
Acylation
Formation of Sulfonic Esters
ad3deb6f5d4dc7823aa3ad2bfe24985be1f3e6860ff8cc0ba215d7624074ef69
ec645297cfd3107bffb1a4753ac125e48856598e58005e939bb2f0e91bf5e57c
O=S(=O)(OCCNc1ccccn1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[C:7]-[C:8](-[OH;D1;+0:9])-[C:10]#[N;D1;H0:11]>>[C:7]-[C:8](-[C:10]#[N;D1;H0:11])-[O;H0;D2;+0:9]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
64.8
[{"value": 64.8, "product": "C1(=CC=C(C=C1)S(=O)(=O)OC(CNC1=NC=C(C=C1)Br)C#N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
7.2 g of 3-(5-bromo-2-pyridinylamino)-2-hydroxypropionitrile was dissolved in 60 mL dichloromethane, and 7.8 mL diisopropyl ethylamine and 6.3 g of 4-toluenesulfonic acid chloride were added thereto, and while the temperature of the mixture was gradually increased to room temperature, the mixture was stirred for 2 hour...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Secondary alcohol.Sulfonyl halide
Tosylate
null
null
c1ccccc1.c1ccncc1
HCl
ClCCl
null
2
Cc1ccc(S(=O)(=O)Cl)cc1.N#CC(O)CNc1ccc(Br)cn1>ClCCl>Cc1ccc(S(=O)(=O)OC(C#N)CNc2ccc(Br)cn2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fa9d214665694c878069c3dfffe8226b
Cc1ccc(S(=O)(=O)OC(C#N)CNc2ccc(Br)cn2)cc1>>N#CC1CN=C2C=CC(Br)=CN21
C1(=CC=C(C=C1)S(=O)(=O)OC(CNC1=NC=C(C=C1)Br)C#N)C>>BrC=1C=CC=2N(C1)C(CN2)C#N
Cc1ccc(S(=O)(=O)O[CH:3]([C:2]#[N:1])[CH2:4][NH:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][n:12]2)cc1>>[N:1]#[C:2][CH:3]1[CH2:4][N:5]=[C:6]2[CH:7]=[CH:8][C:9]([Br:10])=[CH:11][N:12]12
Cc1ccc(S(=O)(=O)OC(C#N)CNc2ccc(Br)cn2)cc1
N#CC1CN=C2C=CC(Br)=CN21
null
null
C(C)#N
Functional Group Interconversion
OtherReaction
dfb00ee5de546e0f8b3b8ef7435d44beb16120a353397d2502be2cb89fa526ee
390a9c1b7a8da6e20e8cfa51452dc793098cd16c7dd6f7fa10ccccabdec3ed20
C1=CC2=NCCN2C=C1
C-c1:c:c:c(-S(=O)(=O)-O-[CH;D3;+0:1](-[C:2]#[N;D1;H0:3])-[C:4]-[NH;D2;+0:5]-[c;H0;D3;+0:6]2:[cH;D2;+0:7]:[cH;D2;+0:8]:[c;H0;D3;+0:9](-[Br;D1;H0:10]):[cH;D2;+0:11]:[n;H0;D2;+0:12]:2):c:c:1>>[Br;D1;H0:10]-[C;H0;D3;+0:9]1=[CH;D2;+0:11]-[N;H0;D3;+0:12]2-[C;H0;D3;+0:6](=[N;H0;D2;+0:5]-[C:4]-[CH;D3;+0:1]-2-[C:2]#[N;D1;H0:3])...
88.7
[{"value": 88.7, "product": "BrC=1C=CC=2N(C1)C(CN2)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7.64 g of 2-(5-bromo-2-pyridinylamino)-1-cyanoethyl toluene-4-sulfonate was dissolved in 76 mL acetonitrile, and the mixture was heated for 15 hours under reflux. After the solvent was removed, an aqueous saturated sodium bicarbonate was poured into the reaction product which was then extracted with dichloromethane, an...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Aromatic halide.Secondary amine
Enamine.Alkenyl halide
c1ccccc1.c1ccncc1
C1=CC2=NCCN2C=C1
C1=CC2=NCCN2C=C1
TsOH.HO-
C(C)#N
null
null
Cc1ccc(S(=O)(=O)OC(C#N)CNc2ccc(Br)cn2)cc1>C(C)#N>N#CC1CN=C2C=CC(Br)=CN21
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b62610f5636e4d9282ac7f4af0117a3c
N#CC1CN=C2C=CC(Br)=CN21>>N#Cc1cnc2ccc(Br)cn12
BrC=1C=CC=2N(C1)C(CN2)C#N.ClC=1C(C(=C(C(C1Cl)=O)C#N)C#N)=O>>BrC=1C=CC=2N(C1)C(=CN2)C#N
[N:1]#[C:2][CH:3]1[CH2:4][N:5]=[C:6]2[CH:7]=[CH:8][C:9]([Br:10])=[CH:11][N:12]12>>[N:1]#[C:2][c:3]1[cH:4][n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][n:12]12
N#CC1CN=C2C=CC(Br)=CN21
N#Cc1cnc2ccc(Br)cn12
null
null
O1CCOCC1.C(C)(=O)OCC
Aromatic Heterocycle Formation
OtherReaction
c60c03c85889124314f6a87395250ea03917b381817a50165cf8f2ae91ef2584
def58fdf0054f9e963777d727e2fcfe02b3d47acb5bb7e18c5e5cf5e7bf2ed6c
c1ccn2ccnc2c1
[Br;D1;H0:1]-[C;H0;D3;+0:2]1=[CH;D2;+0:3]-[N;H0;D3;+0:4]2-[C;H0;D3;+0:5](=[N;H0;D2;+0:6]-[CH2;D2;+0:7]-[CH;D3;+0:8]-2-[C:9]#[N;D1;H0:10])-[CH;D2;+0:11]=[CH;D2;+0:12]-1>>[Br;D1;H0:1]-[c;H0;D3;+0:2]1:[cH;D2;+0:3]:[n;H0;D3;+0:4]2:[c;H0;D3;+0:8](-[C:9]#[N;D1;H0:10]):[cH;D2;+0:7]:[n;H0;D2;+0:6]:[c;H0;D3;+0:5]:2:[cH;D2;+0:11...
85.4
[{"value": 85.4, "product": "BrC=1C=CC=2N(C1)C(=CN2)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Method 1) 3.83 g of 6-bromo-2,3-dihydroimidazo[1,2-a]pyridine-3-carbonitrile synthesized in Production Example 242 was dissolved in 34 mL 1,4-dioxane, and the solution together with 4.3 g of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone was heated at 90° C. for 2 hours. The reaction solution was diluted with ethyl acetate,...
10.6084/m9.figshare.5104873.v1
null
Enamine.Alkenyl halide
Aromatic halide
C1=CC2=NCCN2C=C1
c1ccn2ccnc2c1
c1ccn2ccnc2c1
null
O1CCOCC1.C(C)(=O)OCC
null
null
N#CC1CN=C2C=CC(Br)=CN21>O1CCOCC1.C(C)(=O)OCC>N#Cc1cnc2ccc(Br)cn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7c7fbe84916a4ebe8d9ff238d3978720
Brc1ccc2ncc(I)n2c1.Cc1ccc(S(=O)(=O)C#N)cc1>>N#Cc1cnc2ccc(Br)cn12
O.C1(=CC=C(C=C1)S(=O)(=O)C#N)C.BrC=1C=CC=2N(C1)C(=CN2)I.C(C)(C)[Mg]Br>>BrC=1C=CC=2N(C1)C(=CN2)C#N
I[c:3]1[cH:4][n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][n:12]12.Cc1ccc(S(=O)(=O)[C:2]#[N:1])cc1>>[N:1]#[C:2][c:3]1[cH:4][n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][n:12]12
Brc1ccc2ncc(I)n2c1.Cc1ccc(S(=O)(=O)C#N)cc1
N#Cc1cnc2ccc(Br)cn12
null
null
O1CCCC1.C(C)(=O)OCC
C-C Coupling
OtherReaction
1c185869e396ba40d6e6c73fdf1a72d984b9f87eb77d8ce186cddb8a9f25dc8c
79fb0bb14338c3c783579b68b1bc350a3e7823991438eaa347be0f216d7b34eb
c1ccn2ccnc2c1
C-c1:c:c:c(-S(=O)(=O)-[C;H0;D2;+0:1]#[N;D1;H0:2]):c:c:1.I-[c;H0;D3;+0:3]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[#7;a:8]:1:[c:9]>>[N;D1;H0:2]#[C;H0;D2;+0:1]-[c;H0;D3;+0:3]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[#7;a:8]:1:[c:9]
71.6
[{"value": 71.6, "product": "BrC=1C=CC=2N(C1)C(=CN2)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
Method 2) 80 g of 6-bromo-3-iodoimidazo[1,2-a]pyridine (compound in Production Example 49) was dissolved in 500 mL tetrahydrofuran, and 273 mL of 1.0 M isopropyl magnesium bromide in tetrahydrofuran was slowly added dropwise thereto at 0° C. and stirred for 30 minutes, and 380 mL of 68 g 4-toluenesulfonyl cyanide in te...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Aromatic halide.Nitrile
Nitrile
c1ccn2ccnc2c1.c1ccccc1
c1ccn2ccnc2c1
c1ccn2ccnc2c1
TsOH.HI
O1CCCC1.C(C)(=O)OCC
0
0.5
Brc1ccc2ncc(I)n2c1.Cc1ccc(S(=O)(=O)C#N)cc1>O1CCCC1.C(C)(=O)OCC>N#Cc1cnc2ccc(Br)cn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b25c921be4ca48ae96c29e3739a4f638
COC(=O)c1cnc2ccc(-c3cn(C(c4ccccc4)(c4ccccc4)c4ccccc4)nc3-c3ccc(F)cc3)cn12.NN>>NNC(=O)c1cnc2ccc(-c3cn(C(c4ccccc4)(c4ccccc4)c4ccccc4)nc3-c3ccc(F)cc3)cn12
FC1=CC=C(C=C1)C1=NN(C=C1C=1C=CC=2N(C1)C(=CN2)C(=O)OC)C(C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2.O.NN>>FC1=CC=C(C=C1)C1=NN(C=C1C=1C=CC=2N(C1)C(=CN2)C(=O)NN)C(C2=CC=CC=C2)(C2=CC=CC=C2)C2=CC=CC=C2
CO[C:3](=[O:4])[c:5]1[cH:6][n:7][c:8]2[cH:9][cH:10][c:11](-[c:12]3[cH:13][n:14]([C:15]([c:16]4[cH:17][cH:18][cH:19][cH:20][cH:21]4)([c:22]4[cH:23][cH:24][cH:25][cH:26][cH:27]4)[c:28]4[cH:29][cH:30][cH:31][cH:32][cH:33]4)[n:34][c:35]3-[c:36]3[cH:37][cH:38][c:39]([F:40])[cH:41][cH:42]3)[cH:43][n:44]12.[NH2:1][NH2:2]>>[NH...
COC(=O)c1cnc2ccc(-c3cn(C(c4ccccc4)(c4ccccc4)c4ccccc4)nc3-c3ccc(F)cc3)cn12.NN
NNC(=O)c1cnc2ccc(-c3cn(C(c4ccccc4)(c4ccccc4)c4ccccc4)nc3-c3ccc(F)cc3)cn12
null
null
C(C)O
Acylation
Aminolysis of esters
2e40a14c7d71c6b9001f460fbb953805c923b2db988c8c04f234b9bb5f04424f
3b636feb164ef0f3c8a4f1764f18a25b9eee32ed1463e3bb4b6f1becb871ca74
c1ccc(-c2nn(C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2-c2ccc3nccn3c2)cc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[c:4]:[#7;a:5]:[c:6]:[#7;a:7]:1:[c:8].[N;D1;H2:9]-[NH2;D1;+0:10]>>[N;D1;H2:9]-[NH;D2;+0:10]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[c:4]:[#7;a:5]:[c:6]:[#7;a:7]:1:[c:8]
null
[]
null
null
null
null
A mixture of 740 mg methyl 6-[3-(4-fluorophenyl)-1-trityl-1H-pyrazol-4-yl]imidazo[1,2-a]pyridine-3-carboxylate (compound in Production Example 273), 0.32 mL hydrazine monohydrate and 20 mL ethanol was heated for 6 hours under reflux. The reaction solution was evaporated, and the resulting residue was purified by NH sil...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ester
Acylhydrazine
null
null
c1ccn2ccnc2c1.c1cn[nH]c1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C(C)O
null
null
COC(=O)c1cnc2ccc(-c3cn(C(c4ccccc4)(c4ccccc4)c4ccccc4)nc3-c3ccc(F)cc3)cn12.NN>C(C)O>NNC(=O)c1cnc2ccc(-c3cn(C(c4ccccc4)(c4ccccc4)c4ccccc4)nc3-c3ccc(F)cc3)cn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0bdc1355248043108d099b572644b3e7
Brc1ccc2ncc(I)n2c1.CCOC(=O)Cl>>CCOC(=O)c1cnc2ccc(Br)cn12
C(C)(C)[Mg]Br.C([O-])(O)=O.[Na+].C(OCC)(=O)Cl.BrC=1C=CC=2N(C1)C(=CN2)I>>BrC=1C=CC=2N(C1)C(=CN2)C(=O)OCC
I[c:6]1[cH:7][n:8][c:9]2[cH:10][cH:11][c:12]([Br:13])[cH:14][n:15]12.Cl[C:4]([O:3][CH2:2][CH3:1])=[O:5]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][n:8][c:9]2[cH:10][cH:11][c:12]([Br:13])[cH:14][n:15]12
Brc1ccc2ncc(I)n2c1.CCOC(=O)Cl
CCOC(=O)c1cnc2ccc(Br)cn12
null
null
O1CCCC1.O.C(C)(=O)OCC
C-C Coupling
OtherReaction
d25f86b249f115db5eee10f5e81a0de60ce8996fa162e499c0393c27c8ec46ac
e492b0c20aeea4be57b3b35f202d8ad0bd499fdae4bec30be882f32b4e25bf9b
c1ccn2ccnc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C:4].I-[c;H0;D3;+0:5]1:[c:6]:[#7;a:7]:[c:8](:[c:9]):[#7;a:10]:1:[c:11]>>[C:4]-[#8:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:5]1:[c:6]:[#7;a:7]:[c:8](:[c:9]):[#7;a:10]:1:[c:11]
null
[]
0
CELSIUS
1.5
HOUR
A mixture of 9.69 g 6-bromo-3-iodoimidazo[1,2-a]pyridine (compound in Production Example 49) and 450 mL anhydrous tetrahydrofuran was added little by little to 4.5 mL isopropyl magnesium bromide (0.75 M tetrahydrofuran solution) under ice-cooling in a stream of nitrogen. Then, this reaction solution was returned to roo...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Aromatic halide
Ester
c1ccn2ccnc2c1
c1ccn2ccnc2c1
c1ccn2ccnc2c1
I-
O1CCCC1.O.C(C)(=O)OCC
0
1.5
Brc1ccc2ncc(I)n2c1.CCOC(=O)Cl>O1CCCC1.O.C(C)(=O)OCC>CCOC(=O)c1cnc2ccc(Br)cn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c14ea3baa17245c0a6469ad64bce125d
CCOC(=O)c1cnc2ccc(Br)cn12.NN>>NNC(=O)c1cnc2ccc(Br)cn12
BrC=1C=CC=2N(C1)C(=CN2)C(=O)OCC.O.NN>>BrC=1C=CC=2N(C1)C(=CN2)C(=O)NN
CCO[C:3](=[O:4])[c:5]1[cH:6][n:7][c:8]2[cH:9][cH:10][c:11]([Br:12])[cH:13][n:14]12.[NH2:1][NH2:2]>>[NH2:1][NH:2][C:3](=[O:4])[c:5]1[cH:6][n:7][c:8]2[cH:9][cH:10][c:11]([Br:12])[cH:13][n:14]12
CCOC(=O)c1cnc2ccc(Br)cn12.NN
NNC(=O)c1cnc2ccc(Br)cn12
null
null
C(C)O
Acylation
Aminolysis of esters
2e40a14c7d71c6b9001f460fbb953805c923b2db988c8c04f234b9bb5f04424f
3b636feb164ef0f3c8a4f1764f18a25b9eee32ed1463e3bb4b6f1becb871ca74
c1ccn2ccnc2c1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[c:4]:[#7;a:5]:[c:6]:[#7;a:7]:1:[c:8].[N;D1;H2:9]-[NH2;D1;+0:10]>>[N;D1;H2:9]-[NH;D2;+0:10]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[c:4]:[#7;a:5]:[c:6]:[#7;a:7]:1:[c:8]
null
[]
null
null
null
null
A mixture of 1.94 g ethyl 6-bromoimidazo[1,2-a]pyridine-3-carboxylate, 6 mL hydrazine monohydrate and 20 mL ethanol was heated for 1 hour under reflux. The precipitated crystals were collected by filtration, washed with ethanol and dried under reduced pressure by a vacuum pump to give 1.71 g of the title compound as pa...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ester
Acylhydrazine
null
null
c1ccn2ccnc2c1
HO-
C(C)O
null
null
CCOC(=O)c1cnc2ccc(Br)cn12.NN>C(C)O>NNC(=O)c1cnc2ccc(Br)cn12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6daa03a51b114bf9858fad4788a0195e
COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1.NNC(=O)c1cnc2ccc(Br)cn12.O=C(Cl)C1CC1>>Brc1ccc2ncc(-c3nnc(C4CC4)s3)n2c1
C1(CC1)C(=O)Cl.BrC=1C=CC=2N(C1)C(=CN2)C(=O)NN.C([O-])(O)=O.[Na+].COC=1C=CC(=CC1)P2(=S)SP(=S)(S2)C=3C=CC(=CC3)OC.C1(=CC=CC=C1)C>>BrC=1C=CC=2N(C1)C(=CN2)C=2SC(=NN2)C2CC2
COc1ccc(P2(=S)SP(c3ccc(OC)cc3)(=[S:16])S2)cc1.O=[C:9]([c:8]1[cH:7][n:6][c:5]2[cH:4][cH:3][c:2]([Br:1])[cH:18][n:17]21)[NH:10][NH2:11].O=[C:12](Cl)[CH:13]1[CH2:14][CH2:15]1>>[Br:1][c:2]1[cH:3][cH:4][c:5]2[n:6][cH:7][c:8](-[c:9]3[n:10][n:11][c:12]([CH:13]4[CH2:14][CH2:15]4)[s:16]3)[n:17]2[cH:18]1
COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1.NNC(=O)c1cnc2ccc(Br)cn12.O=C(Cl)C1CC1
Brc1ccc2ncc(-c3nnc(C4CC4)s3)n2c1
null
null
O1CCCC1.O
Miscellaneous
OtherReaction
6e7e92a80e6b5a414388b497b645e527fda43b733f7d88e9222f0050a0b49f09
9a3225718571e61518419c747e141a5e7b98877e2ba2174d3bb27bdb65f706d6
c1ccn2c(-c3nnc(C4CC4)s3)cnc2c1
C-O-c1:c:c:c(-P2(=S)-S-P(=[S;H0;D1;+0:1])(-c3:c:c:c(-O-C):c:c:3)-S-2):c:c:1.Cl-[C;H0;D3;+0:2](=O)-[C:3]1-[C:4]-[C:5]-1.O=[C;H0;D3;+0:6](-[NH;D2;+0:7]-[NH2;D1;+0:8])-[c;H0;D3;+0:9]1:[c:10]:[#7;a:11]:[c:12](:[c:13]):[#7;a:14]:1:[c:15]>>[c:15]:[#7;a:14]1:[c:12](:[c:13]):[#7;a:11]:[c:10]:[c;H0;D3;+0:9]:1-[c;H0;D3;+0:6]1:[n...
null
[]
null
null
8
HOUR
0.22 mL cyclopropane carbonyl chloride was added at room temperature to a mixture of 510 mg 6-bromoimidazo[1,2-a]pyridine-3-carboxylic acid hydrazide (compound in Production Example 276), 202 mg sodium bicarbonate, 15 mL tetrahydrofuran and 15 mL water, and the mixture was stirred overnight. The organic layer was separ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acylhydrazine.Ether.Ether.Monosulfide.Monosulfide
null
c1ccccc1.P1SPS1.c1ccccc1
c1nncs1
c1ccn2ccnc2c1.c1nncs1.C1CC1
HCl
O1CCCC1.O
null
8
COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1.NNC(=O)c1cnc2ccc(Br)cn12.O=C(Cl)C1CC1>O1CCCC1.O>Brc1ccc2ncc(-c3nnc(C4CC4)s3)n2c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d82e24a2be0747a08b3ebbc045c400ba
CI.NNC(=O)c1cnc2ccc(Br)cn12.S=C=S>>CSc1nnc(-c2cnc3ccc(Br)cn23)o1
BrC=1C=CC=2N(C1)C(=CN2)C(=O)NN.[OH-].[Na+].C(=S)=S.CI.C([O-])([O-])=O.[K+].[K+]>>BrC=1C=CC=2N(C1)C(=CN2)C=2OC(=NN2)SC
I[CH3:1].[NH2:4][NH:5][C:6]([c:7]1[cH:8][n:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][n:16]12)=[O:17].S=[C:3]=[S:2]>>[CH3:1][S:2][c:3]1[n:4][n:5][c:6](-[c:7]2[cH:8][n:9][c:10]3[cH:11][cH:12][c:13]([Br:14])[cH:15][n:16]23)[o:17]1
CI.NNC(=O)c1cnc2ccc(Br)cn12.S=C=S
CSc1nnc(-c2cnc3ccc(Br)cn23)o1
null
null
O.CN(C=O)C.C(C)(=O)OCC.C(C)O
Aromatic Heterocycle Formation
OtherReaction
a15f2bb205835a52a07e1d5735ecf8c10312f9f9f9bd5bc3c4fe361d9edeb208
2490f837e85471307bcfdf18fc468adc3367e4e60eef0d0c8d14c76d34701a72
c1ccn2c(-c3nnco3)cnc2c1
I-[CH3;D1;+0:1].S=[C;H0;D2;+0:2]=[S;H0;D1;+0:3].[NH2;D1;+0:4]-[NH;D2;+0:5]-[C;H0;D3;+0:6](=[O;H0;D1;+0:7])-[c;H0;D3;+0:8]1:[c:9]:[#7;a:10]:[c:11](:[c:12]):[#7;a:13]:1:[c:14]>>[CH3;D1;+0:1]-[S;H0;D2;+0:3]-[c;H0;D3;+0:2]1:[n;H0;D2;+0:4]:[n;H0;D2;+0:5]:[c;H0;D3;+0:6](-[c;H0;D3;+0:8]2:[c:9]:[#7;a:10]:[c:11](:[c:12]):[#7;a:...
null
[]
null
null
10
MINUTE
A mixture of 1 g 6-bromoimidazo[1,2-a]pyridine-3-carboxylic acid hydrazide (compound in Production Example 276), 0.24 mL carbon disulfide, 157 mg sodium hydroxide, 15 mL ethanol and 15 mL water was heated for 5 hours under reflux. The reaction solution was poured into a mixture of iced water and an aqueous saturated am...
10.6084/m9.figshare.5104873.v1
null
Acylhydrazine
Monosulfide
null
c1nnco1
c1nnco1.c1ccn2ccnc2c1
HI
O.CN(C=O)C.C(C)(=O)OCC.C(C)O
null
0.166667
CI.NNC(=O)c1cnc2ccc(Br)cn12.S=C=S>O.CN(C=O)C.C(C)(=O)OCC.C(C)O>CSc1nnc(-c2cnc3ccc(Br)cn23)o1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0797dd6832b142a3b1f415dd8aed0253
CSc1nnc(-c2cnc3ccc(Br)cn23)o1>>CS(=O)(=O)c1nnc(-c2cnc3ccc(Br)cn23)o1
ClC1=CC(=CC=C1)C(=O)OO.BrC=1C=CC=2N(C1)C(=CN2)C=2OC(=NN2)SC.ClCCl.S(=S)(=O)([O-])[O-].[Na+].[Na+]>>BrC=1C=CC=2N(C1)C(=CN2)C=2OC(=NN2)S(=O)(=O)C
[CH3:1][S:2][c:5]1[n:6][n:7][c:8](-[c:9]2[cH:10][n:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][n:18]23)[o:19]1>>[CH3:1][S:2](=[O:3])(=[O:4])[c:5]1[n:6][n:7][c:8](-[c:9]2[cH:10][n:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][n:18]23)[o:19]1
CSc1nnc(-c2cnc3ccc(Br)cn23)o1
CS(=O)(=O)c1nnc(-c2cnc3ccc(Br)cn23)o1
null
null
C(C)(=O)OCC
Oxidation
OtherReaction
20dd6d48007b4fe7cd760226f21413eb5e71e6468db112596c2e7ea4858c8ac1
5cedc1bf0f43f21d78a249521ecfcec19fc5ac4895c41eed0e84f0c2618149fa
c1ccn2c(-c3nnco3)cnc2c1
[C;D1;H3:1]-[S;H0;D2;+0:2]-[c:3]1:[#7;a:4]:[#7;a:5]:[c:6]:[#8;a:7]:1>>[C;D1;H3:1]-[S;H0;D4;+0:2](=[O;D1;H0:8])(=[O;D1;H0:9])-[c:3]1:[#7;a:4]:[#7;a:5]:[c:6]:[#8;a:7]:1
null
[]
null
null
8
HOUR
1.16 g of m-chloroperbenzoic acid was added to a mixture of 981 mg 6-bromo-3-(5-methylsulfanyl[1,3,4]oxadiazol-2-yl)imidazo[1,2-a]pyridine (compound in Production Example 279) and 30 mL dichloromethane under ice-coolingd water, then retuned to room temperature and stirred overnight. Ethyl acetate and an aqueous saturat...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfone
null
null
c1nnco1.c1ccn2ccnc2c1
null
C(C)(=O)OCC
null
8
CSc1nnc(-c2cnc3ccc(Br)cn23)o1>C(C)(=O)OCC>CS(=O)(=O)c1nnc(-c2cnc3ccc(Br)cn23)o1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2c35e213c542401e8ac9e4c82950976c
CC(C)O.CS(=O)(=O)c1nnc(-c2cnc3ccc(Br)cn23)o1>>CC(C)Oc1nnc(-c2cnc3ccc(Br)cn23)o1
BrC=1C=CC=2N(C1)C(=CN2)C=2OC(=NN2)S(=O)C.BrC=1C=CC=2N(C1)C(=CN2)C=2OC(=NN2)S(=O)(=O)C.[Cl-].[NH4+].C(C)(C)O>>BrC=1C=CC=2N(C1)C(=CN2)C=2OC(=NN2)OC(C)C
[CH3:1][CH:2]([CH3:3])[OH:4].CS(=O)(=O)[c:5]1[n:6][n:7][c:8](-[c:9]2[cH:10][n:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][n:18]23)[o:19]1>>[CH3:1][CH:2]([CH3:3])[O:4][c:5]1[n:6][n:7][c:8](-[c:9]2[cH:10][n:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][n:18]23)[o:19]1
CC(C)O.CS(=O)(=O)c1nnc(-c2cnc3ccc(Br)cn23)o1
CC(C)Oc1nnc(-c2cnc3ccc(Br)cn23)o1
null
null
O1CCCC1.O.C(C)N(CC)CC.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
8fad2d56540e14e643f6dc70b026544c6d73489f115c0eecdf01048bcbd555ae
470422bbafd7315f89003b23963391a1a49ca3fe240736a0f6aea864ae217419
c1ccn2c(-c3nnco3)cnc2c1
C-S(=O)(=O)-[c;H0;D3;+0:1]1:[#7;a:2]:[#7;a:3]:[c:4](-[c:5](:[#7;a:6]):[c:7]:[#7;a:8]):[#8;a:9]:1.[C;D1;H3:10]-[C:11](-[C;D1;H3:12])-[OH;D1;+0:13]>>[#7;a:8]:[c:7]:[c:5](-[c:4]1:[#7;a:3]:[#7;a:2]:[c;H0;D3;+0:1](-[O;H0;D2;+0:13]-[C:11](-[C;D1;H3:10])-[C;D1;H3:12]):[#8;a:9]:1):[#7;a:6]
null
[]
null
null
null
null
A mixture consisting of 60 mg crude product of a mixture of 6-bromo-3-(5-methanesulfinyl[1,3,4]oxadiazol-2-yl)imidazo[1,2-a]pyridine and 6-bromo-3-(5-methylsulfonyl[1,3,4]oxadiazol-2-yl)imidazo[1,2-a]pyridine obtained in the synthesis process in Production Example 280, 2 mL isopropyl alcohol, 0.3 mL triethylamine and 3...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Sulfone
Ether
c1nnco1
c1nnco1
c1nnco1.c1ccn2ccnc2c1
HO-
O1CCCC1.O.C(C)N(CC)CC.C(C)(=O)OCC
null
null
CC(C)O.CS(=O)(=O)c1nnc(-c2cnc3ccc(Br)cn23)o1>O1CCCC1.O.C(C)N(CC)CC.C(C)(=O)OCC>CC(C)Oc1nnc(-c2cnc3ccc(Br)cn23)o1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-116314e1f49e4302b21416115f54041d
CI.NNC(=O)c1cnc2ccc(Br)cn12.S=C=S>>CSc1nnc(-c2cnc3ccc(Br)cn23)s1
[OH-].[K+].BrC=1C=CC=2N(C1)C(=CN2)C(=O)NN.C(=S)=S.CI.C([O-])(O)=O.[Na+].O.C1(=CC=C(C=C1)S(=O)(=O)O)C>>BrC=1C=CC=2N(C1)C(=CN2)C=2SC(=NN2)SC
I[CH3:1].O=[C:6]([NH:5][NH2:4])[c:7]1[cH:8][n:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][n:16]12.[S:2]=[C:3]=[S:17]>>[CH3:1][S:2][c:3]1[n:4][n:5][c:6](-[c:7]2[cH:8][n:9][c:10]3[cH:11][cH:12][c:13]([Br:14])[cH:15][n:16]23)[s:17]1
CI.NNC(=O)c1cnc2ccc(Br)cn12.S=C=S
CSc1nnc(-c2cnc3ccc(Br)cn23)s1
null
null
O.C1(=CC=CC=C1)C.C(C)(=O)OCC.CO.O1CCCC1
Aromatic Heterocycle Formation
OtherReaction
c5033f81c247361e8d995dd2badb8a8d4561d2b50e44ef1df1a354362b1cc63c
2490f837e85471307bcfdf18fc468adc3367e4e60eef0d0c8d14c76d34701a72
c1ccn2c(-c3nncs3)cnc2c1
I-[CH3;D1;+0:1].O=[C;H0;D3;+0:2](-[NH;D2;+0:3]-[NH2;D1;+0:4])-[c;H0;D3;+0:5]1:[c:6]:[#7;a:7]:[c:8](:[c:9]):[#7;a:10]:1:[c:11].[S;H0;D1;+0:12]=[C;H0;D2;+0:13]=[S;H0;D1;+0:14]>>[CH3;D1;+0:1]-[S;H0;D2;+0:14]-[c;H0;D3;+0:13]1:[n;H0;D2;+0:4]:[n;H0;D2;+0:3]:[c;H0;D3;+0:2](-[c;H0;D3;+0:5]2:[c:6]:[#7;a:7]:[c:8](:[c:9]):[#7;a:1...
5.1
[{"value": 5.1, "product": "BrC=1C=CC=2N(C1)C(=CN2)C=2SC(=NN2)SC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2.5
HOUR
66 mg potassium hydroxide (powder) was added to a mixture of 306 mg of 6-bromoimidazo[1,2-a]pyridine-3-carboxylic acid hydrazide (compound in Production Example 276), 195 mg carbon disulfide and 12 mL methanol under cooling with ice-water, and the mixture was stirred for 2.5 hours. Then, the reaction mixture was return...
10.6084/m9.figshare.5104873.v1
null
Acylhydrazine
Monosulfide
null
c1nncs1
c1nncs1.c1ccn2ccnc2c1
HI
O.C1(=CC=CC=C1)C.C(C)(=O)OCC.CO.O1CCCC1
null
2.5
CI.NNC(=O)c1cnc2ccc(Br)cn12.S=C=S>O.C1(=CC=CC=C1)C.C(C)(=O)OCC.CO.O1CCCC1>CSc1nnc(-c2cnc3ccc(Br)cn23)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ea58fd028a1c48f494e56cfad00eee8d
N#CCCCBr.Sc1cccs1>>N#CCCCSc1cccs1
S1C(=CC=C1)S.BrCCCC#N.C([O-])([O-])=O.[K+].[K+]>>S1C(=CC=C1)SCCCC#N
Br[CH2:5][CH2:4][CH2:3][C:2]#[N:1].[SH:6][c:7]1[cH:8][cH:9][cH:10][s:11]1>>[N:1]#[C:2][CH2:3][CH2:4][CH2:5][S:6][c:7]1[cH:8][cH:9][cH:10][s:11]1
N#CCCCBr.Sc1cccs1
N#CCCCSc1cccs1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
thioether_nucl_sub
26df88c6a3f5f203c89584658be4e126cb42994c98a2e16bc812e1036cdae857
8b2f52296c3a93039174c980b6042ba15754e04d6892a1284c3a32985220b214
c1ccsc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3].[SH;D1;+0:4]-[c:5](:[c:6]):[#16;a:7]:[c:8]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:4]-[c:5](:[c:6]):[#16;a:7]:[c:8]
93.7
[{"value": 93.7, "product": "S1C(=CC=C1)SCCCC#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2.3 g of thiophen-2-thiol, 3.0 g of 4-bromobutyronitrile and 5.5 g of potassium carbonate were stirred in N,N-dimethylformamide at room temperature to give 3.4 g of 4-(2-thienylsulfanyl)butane nitrile. 3.4 g of 4-(2-thienylsulfanyl)butane nitrile was reacted with 5.4 g of N-iodosuccinimide in N,N-dimethylformamide, whe...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic thiol
Monosulfide
null
null
c1ccsc1
HBr
CN(C=O)C
null
null
N#CCCCBr.Sc1cccs1>CN(C=O)C>N#CCCCSc1cccs1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-65f4b916b44c4c289686bb041aa72e0e
N#CCCCSc1cccs1.O=C1CCC(=O)N1I>>N#CCCCSc1ccc(I)s1
S1C(=CC=C1)SCCCC#N.IN1C(CCC1=O)=O>>IC1=CC=C(S1)SCCCC#N
[N:1]#[C:2][CH2:3][CH2:4][CH2:5][S:6][c:7]1[cH:8][cH:9][cH:10][s:12]1.O=C1CCC(=O)N1[I:11]>>[N:1]#[C:2][CH2:3][CH2:4][CH2:5][S:6][c:7]1[cH:8][cH:9][c:10]([I:11])[s:12]1
N#CCCCSc1cccs1.O=C1CCC(=O)N1I
N#CCCCSc1ccc(I)s1
null
null
CN(C=O)C
Functional Group Interconversion
OtherReaction
a42d5393618d10b862dd7bd471fa3f4459c31017c8714cafb4e591f8ed4a8052
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccsc1
O=C1-C-C-C(=O)-N-1-[I;H0;D1;+0:1].[#16;a:2]1:[c:3]:[c:4]:[c:5]:[cH;D2;+0:6]:1>>[I;H0;D1;+0:1]-[c;H0;D3;+0:6]1:[#16;a:2]:[c:3]:[c:4]:[c:5]:1
95.9
[{"value": 95.9, "product": "IC1=CC=C(S1)SCCCC#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2.3 g of thiophen-2-thiol, 3.0 g of 4-bromobutyronitrile and 5.5 g of potassium carbonate were stirred in N,N-dimethylformamide at room temperature to give 3.4 g of 4-(2-thienylsulfanyl)butane nitrile. 3.4 g of 4-(2-thienylsulfanyl)butane nitrile was reacted with 5.4 g of N-iodosuccinimide in N,N-dimethylformamide, whe...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1ccsc1.C1CCNC1
c1ccsc1
c1ccsc1
HO-
CN(C=O)C
null
null
N#CCCCSc1cccs1.O=C1CCC(=O)N1I>CN(C=O)C>N#CCCCSc1ccc(I)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7f4bc2a336c049ec819b1747c7048809
ICI.N#CCCCc1nc2ccc(N)cc2s1>>N#CCCCc1nc2ccc(I)cc2s1
NC1=CC2=C(N=C(S2)CCCC#N)C=C1.N(=O)OCCC(C)C.ICI>>IC1=CC2=C(N=C(S2)CCCC#N)C=C1
IC[I:12].N[c:11]1[cH:10][cH:9][c:8]2[n:7][c:6]([CH2:5][CH2:4][CH2:3][C:2]#[N:1])[s:15][c:14]2[cH:13]1>>[N:1]#[C:2][CH2:3][CH2:4][CH2:5][c:6]1[n:7][c:8]2[cH:9][cH:10][c:11]([I:12])[cH:13][c:14]2[s:15]1
ICI.N#CCCCc1nc2ccc(N)cc2s1
N#CCCCc1nc2ccc(I)cc2s1
null
[Cu]I
O1CCCC1
Functional Group Interconversion
OtherReaction
19efdc3671eccba483079778163c471f0ac1c0cc2cc14e140c8bd1068411c52f
a511902c9d47eba7e9fb55f1fce242c65253f2ae6cd2fe001fbf65238d3d696d
c1ccc2scnc2c1
I-C-[I;H0;D1;+0:1].N-[c;H0;D3;+0:2]1:[c:3]:[c:4]:[c:5]2:[#7;a:6]:[c:7]:[#16;a:8]:[c:9]:2:[c:10]:1>>[I;H0;D1;+0:1]-[c;H0;D3;+0:2]1:[c:3]:[c:4]:[c:5]2:[#7;a:6]:[c:7]:[#16;a:8]:[c:9]:2:[c:10]:1
null
[]
null
null
null
null
1.1 g of 4-(6-amino-1,3-benzothiazol-2-yl)butane nitrile synthesized according to a method described in JP-A 5–194440, 2 mL isoamyl nitrite, 0.96 g of copper (I) iodide and 2 mL diiodomethane were heated in tetrahydrofuran at 80° C. for 1 hour. After the solvent was removed, the residue was purified by NH silica gel co...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Primary amine
Aromatic halide
c1ccc2scnc2c1
c1ccc2scnc2c1
c1ccc2scnc2c1
HI
[Cu]I.O1CCCC1
null
null
ICI.N#CCCCc1nc2ccc(N)cc2s1>[Cu]I.O1CCCC1>N#CCCCc1nc2ccc(I)cc2s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d4ee081e2c314b2999239ecf24ab5827
NC(=O)CC[C@H](O)c1nc2ccc(I)cc2s1>>N#CCC[C@H](O)c1nc2ccc(I)cc2s1
O.N1=CC=CC=C1.FC(C(=O)OC(C(F)(F)F)=O)(F)F.O[C@@H](CCC(=O)N)C=1SC2=C(N1)C=CC(=C2)I>>O[C@@H](CCC#N)C=1SC2=C(N1)C=CC(=C2)I
O=[C:2]([NH2:1])[CH2:3][CH2:4][C@H:5]([OH:6])[c:7]1[n:8][c:9]2[cH:10][cH:11][c:12]([I:13])[cH:14][c:15]2[s:16]1>>[N:1]#[C:2][CH2:3][CH2:4][C@H:5]([OH:6])[c:7]1[n:8][c:9]2[cH:10][cH:11][c:12]([I:13])[cH:14][c:15]2[s:16]1
NC(=O)CC[C@H](O)c1nc2ccc(I)cc2s1
N#CCC[C@H](O)c1nc2ccc(I)cc2s1
null
null
O1CCCC1
Miscellaneous
OtherReaction
5094e9d814705bbdc421edbf7e9198e499e70e93916e2cec6eefbc82d1ba5440
32b9893bcb5223559a9d02852f8392cf6473aacfb044a52ba4e9cb9c29edb170
c1ccc2scnc2c1
O=[C;H0;D3;+0:1](-[NH2;D1;+0:2])-[C:3]-[C:4]>>[C:4]-[C:3]-[C;H0;D2;+0:1]#[N;H0;D1;+0:2]
73.8
[{"value": 73.8, "product": "O[C@@H](CCC#N)C=1SC2=C(N1)C=CC(=C2)I", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
0.33 mL trifluoroacetic anhydride was added to a solution of 556 mg of (4S)-4-hydroxy-4-(6-iodo-1,3-benzothiazol-2-yl)butane amide obtained in Production Example 299 and 0.25 mL pyridine in tetrahydrofuran under ice-cooling, and the mixture was stirred for 2 hours. Water was added thereto, the reaction solution was the...
10.6084/m9.figshare.5104873.v1
null
Primary amide
Nitrile
null
null
c1ccc2scnc2c1
HO-
O1CCCC1
null
2
NC(=O)CC[C@H](O)c1nc2ccc(I)cc2s1>O1CCCC1>N#CCC[C@H](O)c1nc2ccc(I)cc2s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-52e3b9d8c58f45aca3d21a2fe05817b7
C[Si](C)(C)C=[N+]=[N-].Cc1csc(N)n1.O=S(=O)(Cl)c1ccc(I)cc1>>Cc1csc(N(C)S(=O)(=O)c2ccc(I)cc2)n1
IC1=CC=C(C=C1)S(=O)(=O)Cl.NC=1SC=C(N1)C.C[Si](C)(C)C=[N+]=[N-]>>CN(S(=O)(=O)C1=CC=C(C=C1)I)C=1SC=C(N1)C
C[Si](C)(C)[CH:7]=[N+]=[N-].[CH3:1][c:2]1[cH:3][s:4][c:5]([NH2:6])[n:18]1.Cl[S:8](=[O:9])(=[O:10])[c:11]1[cH:12][cH:13][c:14]([I:15])[cH:16][cH:17]1>>[CH3:1][c:2]1[cH:3][s:4][c:5]([N:6]([CH3:7])[S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][c:14]([I:15])[cH:16][cH:17]2)[n:18]1
C[Si](C)(C)C=[N+]=[N-].Cc1csc(N)n1.O=S(=O)(Cl)c1ccc(I)cc1
Cc1csc(N(C)S(=O)(=O)c2ccc(I)cc2)n1
null
null
N1=CC=CC=C1.O1CCCC1.CO
Heteroatom Alkylation and Arylation
OtherReaction
816d3dc285e0587d41466c78207a62d612d2f7a200de0e754a8cfb5e6b1d9bdc
1b91dcd2bb04ce245a0a4cf680c1f998a98b34b516c56e0362ff42c38535ac5c
O=S(=O)(Nc1nccs1)c1ccccc1
C-[Si](-C)(-C)-[CH;D2;+0:1]=[N+]=[N-].Cl-[S;H0;D4;+0:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c:5](:[c:6]):[c:7].[NH2;D1;+0:8]-[c:9]1:[#16;a:10]:[c:11]:[c:12]:[#7;a:13]:1>>[CH3;D1;+0:1]-[N;H0;D3;+0:8](-[c:9]1:[#16;a:10]:[c:11]:[c:12]:[#7;a:13]:1)-[S;H0;D4;+0:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c:5](:[c:6]):[c:7]
null
[]
null
null
1
HOUR
760 mg of N1-(4-methyl-1,3-thiazol-2-yl)-4-iodo-1-benzene sulfonamide obtained by reacting 4-iodobenzenesulfonyl chloride with 2-amino-4-methylthiazole in pyridine was dissolved in a solvent mixture of 5 mL methanol and 3 mL tetrahydrofuran, then 1.1 mL (trimethylsilyl)diazomethane (2 M hexane solution) was added there...
10.6084/m9.figshare.5104873.v1
null
Diazo.Primary amine.Sulfonyl halide.Silyl protective group
Tertiary amine
null
null
c1cscn1.c1ccccc1
HCl
N1=CC=CC=C1.O1CCCC1.CO
null
1
C[Si](C)(C)C=[N+]=[N-].Cc1csc(N)n1.O=S(=O)(Cl)c1ccc(I)cc1>N1=CC=CC=C1.O1CCCC1.CO>Cc1csc(N(C)S(=O)(=O)c2ccc(I)cc2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-378eecc8f6da43fc94723245ce7e7e3f
Cc1csc(N)n1.O=C(O)c1ccc(-c2cnc3ccc(Br)cn23)cc1>>Cc1csc(NC(=O)c2ccc(-c3cnc4ccc(Br)cn34)cc2)n1
BrC=1C=CC=2N(C1)C(=CN2)C2=CC=C(C(=O)O)C=C2.NC=1SC=C(N1)C.F[P-](F)(F)(F)(F)F.N1(N=NC2=C1C=CC=C2)O[P+](N(C)C)(N(C)C)N(C)C.C(C)N(CC)CC>>CC=1N=C(SC1)NC(C1=CC=C(C=C1)C1=CN=C2N1C=C(C=C2)Br)=O
[CH3:1][c:2]1[cH:3][s:4][c:5]([NH2:6])[n:25]1.O[C:7](=[O:8])[c:9]1[cH:10][cH:11][c:12](-[c:13]2[cH:14][n:15][c:16]3[cH:17][cH:18][c:19]([Br:20])[cH:21][n:22]23)[cH:23][cH:24]1>>[CH3:1][c:2]1[cH:3][s:4][c:5]([NH:6][C:7](=[O:8])[c:9]2[cH:10][cH:11][c:12](-[c:13]3[cH:14][n:15][c:16]4[cH:17][cH:18][c:19]([Br:20])[cH:21][n:...
Cc1csc(N)n1.O=C(O)c1ccc(-c2cnc3ccc(Br)cn23)cc1
Cc1csc(NC(=O)c2ccc(-c3cnc4ccc(Br)cn34)cc2)n1
null
null
ClCCl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(Nc1nccs1)c1ccc(-c2cnc3ccccn23)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[NH2;D1;+0:6]-[c:7]1:[#16;a:8]:[c:9]:[c:10]:[#7;a:11]:1>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[NH;D2;+0:6]-[c:7]1:[#16;a:8]:[c:9]:[c:10]:[#7;a:11]:1)-[c:3](:[c:4]):[c:5]
48.3
[{"value": 48.3, "product": "CC=1N=C(SC1)NC(C1=CC=C(C=C1)C1=CN=C2N1C=C(C=C2)Br)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
159 mg of 4-(6-bromoimidazo[1,2-a]pyridin-3-yl)benzoic acid (compound in Production Example 54), 58 mg of 2-amino-4-methyl-1,3-thiazole, 243 mg benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate and 83 μL triethylamine were reacted overnight in 4 mL dichloromethane. The reaction solution was purifi...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1cscn1.c1ccccc1.c1ccn2ccnc2c1
HO-
ClCCl
null
null
Cc1csc(N)n1.O=C(O)c1ccc(-c2cnc3ccc(Br)cn23)cc1>ClCCl>Cc1csc(NC(=O)c2ccc(-c3cnc4ccc(Br)cn34)cc2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7d51ffea0f444886a4623476d3e4569f
CON(C)C(=O)[C@H](C)NC(=O)OC(C)(C)C.Fc1ccc(Br)cc1>>C[C@H](NC(=O)OC(C)(C)C)C(=O)c1ccc(F)cc1
CON(C([C@H](C)NC(OC(C)(C)C)=O)=O)C.BrC1=CC=C(C=C1)F.[Mg].[Cl-].[NH4+]>>FC1=CC=C(C=C1)C([C@H](C)NC(OC(C)(C)C)=O)=O
CON(C)[C:11]([C@H:2]([CH3:1])[NH:3][C:4](=[O:5])[O:6][C:7]([CH3:8])([CH3:9])[CH3:10])=[O:12].Br[c:13]1[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]1>>[CH3:1][C@H:2]([NH:3][C:4](=[O:5])[O:6][C:7]([CH3:8])([CH3:9])[CH3:10])[C:11](=[O:12])[c:13]1[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]1
CON(C)C(=O)[C@H](C)NC(=O)OC(C)(C)C.Fc1ccc(Br)cc1
C[C@H](NC(=O)OC(C)(C)C)C(=O)c1ccc(F)cc1
null
null
O1CCCC1
C-C Coupling
OtherReaction
99face78a8bbaa38ff4dd2141c4a0df3e690005988b6fb5a9a2afc6a90da7e24
7d9aa59f8ecc532475d910f9ab122332ecbb7f9444a37371b7c1bac80798d342
c1ccccc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].C-O-N(-C)-[C;H0;D3;+0:6](=[O;D1;H0:7])-[C:8](-[C;D1;H3:9])-[#7:10]-[C:11](=[O;D1;H0:12])-[#8:13]-[C:14](-[C;D1;H3:15])(-[C;D1;H3:16])-[C;D1;H3:17]>>[C;D1;H3:15]-[C:14](-[C;D1;H3:16])(-[C;D1;H3:17])-[#8:13]-[C:11](=[O;D1;H0:12])-[#7:10]-[C:8](-[C;D1;H3:9])-[C;H0;D3;+0:6](=[O;D...
97.4
[{"value": 97.4, "product": "FC1=CC=C(C=C1)C([C@H](C)NC(OC(C)(C)C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
5
CELSIUS
2
HOUR
A solution of 2.32 g t-butyl N-{(1S)-2-[methoxy(methyl)amino]-1-methyl-2-oxoethyl}carbamate in tetrahydrofuran was added dropwise under ice-cooling to a tetrahydrofuran solution of Grignard reagent prepared from 5.2 g of 1-bromo-4-fluorobenzene and 1 g magnesium. The mixture was stirred at 5° C. for 2 hours, then poure...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tertiary amide
Ketone
c1ccccc1
c1ccccc1
c1ccccc1
HBr
O1CCCC1
5
2
CON(C)C(=O)[C@H](C)NC(=O)OC(C)(C)C.Fc1ccc(Br)cc1>O1CCCC1>C[C@H](NC(=O)OC(C)(C)C)C(=O)c1ccc(F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-de9f6a334b8946788a458cefe95465ad
CSc1cccc(N)c1.O=C(O)c1ccc(Br)cc1F>>CSc1cccc(NC(=O)c2ccc(Br)cc2F)c1
BrC1=CC(=C(C(=O)O)C=C1)F.CSC=1C=C(N)C=CC1>>CSC=1C=C(C=CC1)NC(C1=C(C=C(C=C1)Br)F)=O
[CH3:1][S:2][c:3]1[cH:4][cH:5][cH:6][c:7]([NH2:8])[cH:19]1.O[C:9](=[O:10])[c:11]1[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]1[F:18]>>[CH3:1][S:2][c:3]1[cH:4][cH:5][cH:6][c:7]([NH:8][C:9](=[O:10])[c:11]2[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]2[F:18])[cH:19]1
CSc1cccc(N)c1.O=C(O)c1ccc(Br)cc1F
CSc1cccc(NC(=O)c2ccc(Br)cc2F)c1
null
null
null
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(Nc1ccccc1)c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[NH2;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9])-[c:3](:[c:4]):[c:5]
null
[]
null
null
null
null
460 mg of N1-[3-(methylsulfanyl)phenyl]-4-bromo-2-fluorobenzamide obtained in the same manner as in Production Example 32 from 4-bromo-2-fluorobenzoic acid and 3-(methylthio)aniline was stirred for 1.5 hours together with 1.23 g oxone in 15 mL tetrahydrofuran, 10 mL methanol and 10 mL water. The reaction solution was e...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccccc1
HO-
null
null
null
CSc1cccc(N)c1.O=C(O)c1ccc(Br)cc1F>>CSc1cccc(NC(=O)c2ccc(Br)cc2F)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-95d13c917d1e465a99ea0479340b0bfb
C=[CH][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.Nc1ccc(Br)cn1>>C=Cc1ccc(N)nc1
BrC=1C=CC(=NC1)N.C(CCC)[Sn](C=C)(CCCC)CCCC>>C(=C)C=1C=CC(=NC1)N
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH:2]=[CH2:1].Br[c:3]1[cH:4][cH:5][c:6]([NH2:7])[n:8][cH:9]1>>[CH2:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([NH2:7])[n:8][cH:9]1
C=[CH][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.Nc1ccc(Br)cn1
C=Cc1ccc(N)nc1
null
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1
C=1(C(=CC=CC1)C)C
C-C Coupling
Stille reaction_vinyl
3dd1babd20b217bb4acf07044a72bf65da3bd9404d25a4b198b8fddcb5d9092e
ec03c739f58696d2a3659a73884744e1a490a20a587da6f115be382b663cf23d
c1ccncc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1.C-C-C-[CH2]-[Sn](-[CH2]-C-C-C)(-[CH2]-C-C-C)-[CH;D2;+0:7]=[C;D1;H2:8]>>[C;D1;H2:8]=[CH;D2;+0:7]-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1
45.3
[{"value": 45.3, "product": "C(=C)C=1C=CC(=NC1)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4.13 g 5-bromopyridin-2-yl amine, 7.95 g tributyl(vinyl)tin and 1.38 g tetrakis(triphenylphosphine)palladium were heated in 70 mL xylene at 120° C. for 3 hours under nitrogen atmosphere. The solvent was removed, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate), to give 1.3 g of th...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Vinyl.Tin
Vinyl
c1ccncc1
c1ccncc1
c1ccncc1
HBr.Sn
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.C=1(C(=CC=CC1)C)C
null
null
C=[CH][Sn]([CH2]CCC)([CH2]CCC)[CH2]CCC.Nc1ccc(Br)cn1>C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.C=1(C(=CC=CC1)C)C>C=Cc1ccc(N)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-09aab869bb414c14b748af51fb8fca97
C=Cc1ccc(N)nc1>>CCc1ccc(N)nc1
C(=C)C=1C=CC(=NC1)N>>C(C)C=1C=CC(=NC1)N
[CH2:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([NH2:7])[n:8][cH:9]1>>[CH3:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([NH2:7])[n:8][cH:9]1
C=Cc1ccc(N)nc1
CCc1ccc(N)nc1
null
[C].[Pd]
C(C)(=O)OCC
Reduction
Hydrogenation (double to single)
8276b4fb5ddc7d15dec6d92474e91e2dbb2fb8b81e5b5720762e5d89cb27aa69
1ccae9f2e86499601fc3421041ff4588c8e6fd53048e86c3b6ed12ae873609c0
c1ccncc1
[CH2;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[CH3;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
94.4
[{"value": 94.4, "product": "C(C)C=1C=CC(=NC1)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
0.25 g 5-vinylpyridin-2-yl amine (compound in Production Example 326) and 0.1 g of 10% palladium-carbon were stirred in 5 mL ethyl acetate at room temperature for 2 hours under hydrogen atmosphere. The reaction solution was purified by NH silica gel column chromatography (ethyl acetate), to give 0.24 g of the title com...
10.6084/m9.figshare.5104873.v1
null
Vinyl
null
null
null
c1ccncc1
null
[C].[Pd].C(C)(=O)OCC
null
null
C=Cc1ccc(N)nc1>[C].[Pd].C(C)(=O)OCC>CCc1ccc(N)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ceab4b5f989746cf9e16193cc124bb05
CCOC(=O)c1ccc(Br)cc1F.Nc1ccccc1[N+](=O)[O-]>>CCOC(=O)c1ccc(Nc2ccccc2[N+](=O)[O-])cc1F
BrC1=CC(=C(C(=O)OCC)C=C1)F.[N+](=O)([O-])C1=C(N)C=CC=C1.C([O-])([O-])=O.[Cs+].[Cs+].C1(=CC=CC=C1)C>>FC1=C(C(=O)OCC)C=CC(=C1)NC1=C(C=CC=C1)[N+](=O)[O-]
Br[c:9]1[cH:8][cH:7][c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:21]([F:22])[cH:20]1.[NH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][c:16]1[N+:17](=[O:18])[O-:19]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([NH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[N+:17](=[O:18])[O-:19])[cH:20][c:21]1[F:22]
CCOC(=O)c1ccc(Br)cc1F.Nc1ccccc1[N+](=O)[O-]
CCOC(=O)c1ccc(Nc2ccccc2[N+](=O)[O-])cc1F
null
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C1(=CC=CC=C1)P(C1=C(C2=CC=CC=C2C=C1)C1=C(C=CC2=CC=CC=C12)P(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=CC=C1
O
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(Nc2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[NH2;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[c:8]:[c:7](-[NH;D2;+0:6]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:9]
77.1
[{"value": 77.1, "product": "FC1=C(C(=O)OCC)C=CC(=C1)NC1=C(C=CC=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
1.0 g ethyl 4-bromo-2-fluorobenzoate, 0.56 g 2-nitroaniline, 1.85 g cesium carbonate, 37 mg tris(dibenzylideneacetone)-dipalladium (0), 38 mg 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (racemic mixture) and 15 mL toluene were stirred at 100° C. for 24 hours under nitrogen atmosphere. Water was added thereto, then the ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HBr
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C1(=CC=CC=C1)P(C1=C(C2=CC=CC=C2C=C1)C1=C(C=CC2=CC=CC=C12)P(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=CC=C1.O
null
null
CCOC(=O)c1ccc(Br)cc1F.Nc1ccccc1[N+](=O)[O-]>C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C1(=CC=CC=C1)P(C1=C(C2=CC=CC=C2C=C1)C1=C(C=CC2=CC=CC=C12)P(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=CC=C1.O>CCOC(=O)c1ccc(Nc2ccccc2[N+](=O)[O-])cc1F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bbef1b1f3ba844cbbbb945a5c679fabc
CCOC(=O)c1ccc(Nc2ccccc2[N+](=O)[O-])cc1F>>CCOC(=O)c1ccc(Nc2ccccc2N)cc1F
FC1=C(C(=O)OCC)C=CC(=C1)NC1=C(C=CC=C1)[N+](=O)[O-].[Cl-].[NH4+].CO>>NC1=C(C=CC=C1)NC1=CC(=C(C(=O)OCC)C=C1)F
O=[N+:17]([O-])[c:16]1[c:11]([NH:10][c:9]2[cH:8][cH:7][c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[c:19]([F:20])[cH:18]2)[cH:12][cH:13][cH:14][cH:15]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([NH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[NH2:17])[cH:18][c:19]1[F:20]
CCOC(=O)c1ccc(Nc2ccccc2[N+](=O)[O-])cc1F
CCOC(=O)c1ccc(Nc2ccccc2N)cc1F
null
[Fe]
O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(Nc2ccccc2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
99.3
[{"value": 99.3, "product": "NC1=C(C=CC=C1)NC1=CC(=C(C(=O)OCC)C=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
1
HOUR
200 mg ethyl 2-fluoro-4-(2-nitrophenylamino)benzoate (compound in Production Example 331), 180 mg iron powder, 350 mg ammonium chloride and 8 mL solution mixture of methanol and water (5:3) were stirred at 100° C. for 1 hour. Insolubles were filtered off with Celite, and water was added to the filtrate which was then e...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccccc1
Other
[Fe].O
100
1
CCOC(=O)c1ccc(Nc2ccccc2[N+](=O)[O-])cc1F>[Fe].O>CCOC(=O)c1ccc(Nc2ccccc2N)cc1F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f76b2293b0184ea5b1efefeb0b0b4eb7
CCOC(=O)c1ccc(Nc2ccccc2N)cc1F.O=C1CCC(=O)N1Br>>CCOC(=O)c1ccc(Nc2cc(Br)ccc2N)cc1F
BrN1C(CCC1=O)=O.NC1=C(C=CC=C1)NC1=CC(=C(C(=O)OCC)C=C1)F.S(=S)(=O)([O-])[O-].[Na+].[Na+].C([O-])(O)=O.[Na+]>>NC1=C(C=C(C=C1)Br)NC1=CC(=C(C(=O)OCC)C=C1)F
[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([NH:10][c:11]2[cH:12][cH:13][cH:15][cH:16][c:17]2[NH2:18])[cH:19][c:20]1[F:21].O=C1CCC(=O)N1[Br:14]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([NH:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[NH2:18])[cH:19][c:20]1[F:21]
CCOC(=O)c1ccc(Nc2ccccc2N)cc1F.O=C1CCC(=O)N1Br
CCOC(=O)c1ccc(Nc2cc(Br)ccc2N)cc1F
null
null
CN(C=O)C
Functional Group Interconversion
Bromination
48c1dcf50945076da40bbd7976060ec1ea74b3478ef8c25d67664232b218095c
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccc(Nc2ccccc2)cc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[c:2]:[c:3]:[cH;D2;+0:4]:[c:5]:[c:6]>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:4](:[c:3]:[c:2]):[c:5]:[c:6]
68.2
[{"value": 68.2, "product": "NC1=C(C=C(C=C1)Br)NC1=CC(=C(C(=O)OCC)C=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
179 mg ethyl 4-(2-amino-phenylamino)-2-fluoro-benzoate (compound in Production Example 332) was dissolved in 4 mL N,N-dimethylformamide, and 116 mg N-bromosuccinimide was added thereto under ice-cooling and stirred for 2 hours. An aqueous sodium thiosulfate solution and an aqueous sodium bicarbonate solution were added...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1ccccc1.C1CCNC1
c1ccccc1
c1ccccc1.c1ccccc1
HO-
CN(C=O)C
null
2
CCOC(=O)c1ccc(Nc2ccccc2N)cc1F.O=C1CCC(=O)N1Br>CN(C=O)C>CCOC(=O)c1ccc(Nc2cc(Br)ccc2N)cc1F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a61b24039bde45f7abef76817ce1bb39
CCOC(=O)c1ccc(Nc2cc(Br)ccc2N)cc1F>>CCOC(=O)c1ccc(-n2cnc3ccc(Br)cc32)cc1F
NC1=C(C=C(C=C1)Br)NC1=CC(=C(C(=O)OCC)C=C1)F.C(C)OC(OCC)OCC>>BrC=1C=CC2=C(N(C=N2)C2=CC(=C(C(=O)OCC)C=C2)F)C1
[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([NH:10][c:19]2[c:13]([NH2:12])[cH:14][cH:15][c:16]([Br:17])[cH:18]2)[cH:20][c:21]1[F:22]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9](-[n:10]2[cH:11][n:12][c:13]3[cH:14][cH:15][c:16]([Br:17])[cH:18][c:19]23)[cH:20][c:21]1[F:22]
CCOC(=O)c1ccc(Nc2cc(Br)ccc2N)cc1F
CCOC(=O)c1ccc(-n2cnc3ccc(Br)cc32)cc1F
null
null
null
Aromatic Heterocycle Formation
OtherReaction
d9700fa3e76550743d6e0392726c4e3536c554578499775d8c87d842c6d8bad6
c12bf4e666f812d0e692aca3756678364265d1c8b3469e9563c84f9ed1df94d2
c1ccc(-n2cnc3ccccc32)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4](-[NH;D2;+0:5]-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:11]>>[c:3]:[c:2]1:[n;H0;D2;+0:1]:[c:12]:[n;H0;D3;+0:5](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:1:[c:11]
null
[]
null
null
null
null
917 mg ethyl 4-(2-amino-5-bromo-phenylamino)-2-fluoro-benzoate (compound in Production Example 333) and 7 mL triethoxymethane were stirred at 140° C. for 3 hours. The solvent was evaporated, and the residue was purified by NH silica gel chromatography (ethyl acetate/hexane). By recrystallization from ethyl acetate/hexa...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Secondary amine
null
c1ccccc1
c1ccc2nc[nH]c2c1
c1ccccc1.c1ccc2nc[nH]c2c1
Other
null
null
null
CCOC(=O)c1ccc(Nc2cc(Br)ccc2N)cc1F>>CCOC(=O)c1ccc(-n2cnc3ccc(Br)cc32)cc1F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-969424eeab0d4d7bac8784b2fdc5b2ac
O=[N+]([O-])c1cc(Br)ccc1F>>Nc1cc(Br)ccc1F
BrC=1C=CC(=C(C1)[N+](=O)[O-])F.[Cl-].[NH4+].CO>>BrC=1C=CC(=C(C1)N)F
O=[N+:1]([O-])[c:2]1[cH:3][c:4]([Br:5])[cH:6][cH:7][c:8]1[F:9]>>[NH2:1][c:2]1[cH:3][c:4]([Br:5])[cH:6][cH:7][c:8]1[F:9]
O=[N+]([O-])c1cc(Br)ccc1F
Nc1cc(Br)ccc1F
null
[Fe]
O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccccc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
93.8
[{"value": 93.8, "product": "BrC=1C=CC(=C(C1)N)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
3.0 g of 5-bromo-2-fluoronitrobenzene, 3.8 g iron powder and 7.3 g ammonium chloride were heated at 80° C. for 2 hours in a solution mixture of 30 mL methanol and 30 mL water. The reaction mixture was filtered through Celite, the methanol was evaporated, and the reaction mixture was diluted with water and extracted wit...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1
Other
[Fe].O
null
null
O=[N+]([O-])c1cc(Br)ccc1F>[Fe].O>Nc1cc(Br)ccc1F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cbb7fc0bd2bb4f25abd04ac36e999884
Nc1cc(Br)ccc1F.O=C(c1ccccc1)c1ccccc1>>Fc1ccc(Br)cc1N=C(c1ccccc1)c1ccccc1
BrC=1C=CC(=C(C1)N)F.C(C1=CC=CC=C1)(=O)C1=CC=CC=C1.C1(=CC=C(C=C1)S(=O)(=O)O)C>>C(C1=CC=CC=C1)(C1=CC=CC=C1)=NC1=C(C=CC(=C1)Br)F
[F:1][c:2]1[cH:3][cH:4][c:5]([Br:6])[cH:7][c:8]1[NH2:9].O=[C:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1>>[F:1][c:2]1[cH:3][cH:4][c:5]([Br:6])[cH:7][c:8]1[N:9]=[C:10]([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1
Nc1cc(Br)ccc1F.O=C(c1ccccc1)c1ccccc1
Fc1ccc(Br)cc1N=C(c1ccccc1)c1ccccc1
null
null
C1(=CC=CC=C1)C.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
Addition of primary amines to ketones/thiocarbonyls
cb968592dec1a2c40e9f51052b6ef3c2d7edca4da22c8c4bb0fad7e1c1c69433
009cc6a97ebe0dc96c669f0ef59b95bcc20de7cae20b1b648ce8f8fa82309e57
c1ccc(N=C(c2ccccc2)c2ccccc2)cc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4])-[c:5](:[c:6]):[c:7].[NH2;D1;+0:8]-[c:9](:[c:10]):[c:11]>>[c:3]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:8]-[c:9](:[c:10]):[c:11])-[c:5](:[c:6]):[c:7]):[c:4]
42.2
[{"value": 42.2, "product": "C(C1=CC=CC=C1)(C1=CC=CC=C1)=NC1=C(C=CC(=C1)Br)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
While a solution of 2.43 g 5-bromo-2-fluorophenylamine (compound in Production Example 335), 2.6 g benzophenone and 122 mg 4-toluenesulfonic acid in 50 ml toluene was azeotropically dehydrated, the mixture was heated for 6 hours under reflux. The reaction mixture was diluted with ethyl acetate and washed with brine, th...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
Substituted imine
null
null
c1ccccc1.c1ccccc1.c1ccccc1
HO-
C1(=CC=CC=C1)C.C(C)(=O)OCC
null
null
Nc1cc(Br)ccc1F.O=C(c1ccccc1)c1ccccc1>C1(=CC=CC=C1)C.C(C)(=O)OCC>Fc1ccc(Br)cc1N=C(c1ccccc1)c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-af4e17e2607c4f4c8090d6044bb03da1
CSC.Fc1ccc(Br)cc1N=C(c1ccccc1)c1ccccc1>>CSc1ccc(F)c(N=C(c2ccccc2)c2ccccc2)c1
[Cl-].[NH4+].C(CCC)[Li].C(C1=CC=CC=C1)(C1=CC=CC=C1)=NC1=C(C=CC(=C1)Br)F.CSC>>C(C1=CC=CC=C1)(C1=CC=CC=C1)=NC1=C(C=CC(=C1)SC)F
C[S:2][CH3:1].Br[c:3]1[cH:4][cH:5][c:6]([F:7])[c:8]([N:9]=[C:10]([c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[cH:23]1>>[CH3:1][S:2][c:3]1[cH:4][cH:5][c:6]([F:7])[c:8]([N:9]=[C:10]([c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[cH:23]1
CSC.Fc1ccc(Br)cc1N=C(c1ccccc1)c1ccccc1
CSc1ccc(F)c(N=C(c2ccccc2)c2ccccc2)c1
null
null
O1CCCC1.O
Heteroatom Alkylation and Arylation
OtherReaction
8c6dc51512ab28d4cb9441689ce7cb87249900712ea999d5c69c20b93d2b2353
c58e6934d5c82ddec3b0774dc166fdbb9c9ad3acfbb76cde182cbe53c5c1e68c
c1ccc(N=C(c2ccccc2)c2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].C-[S;H0;D2;+0:6]-[C;D1;H3:7]>>[C;D1;H3:7]-[S;H0;D2;+0:6]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
15
MINUTE
2.2 mL n-butyl lithium (2.66 M hexane solution) was added dropwise to a solution of 1.85 g benzhydrylidene-(5-bromo-2-fluorophenyl)-amine (compound in Production Example 336) in 10 mL tetrahydrofuran at −70° C., then the mixture was stirred for 15 minutes, a solution of 0.53 mL methyl sulfide in 5 mL tetrahydrofuran wa...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Monosulfide
Monosulfide
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1
HBr
O1CCCC1.O
null
0.25
CSC.Fc1ccc(Br)cc1N=C(c1ccccc1)c1ccccc1>O1CCCC1.O>CSc1ccc(F)c(N=C(c2ccccc2)c2ccccc2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-301e0a8a384a44118b2bb5ca131ee775
CS(=O)(=O)c1ccc(F)c(N)c1.ClCCNCCCl>>CS(=O)(=O)c1ccc(F)c(N2CCNCC2)c1
C([O-])(O)=O.[Na+].FC1=C(C=C(C=C1)S(=O)(=O)C)N.Cl.ClCCNCCCl>>FC1=C(C=C(C=C1)S(=O)(=O)C)N1CCNCC1
[CH3:1][S:2](=[O:3])(=[O:4])[c:5]1[cH:6][cH:7][c:8]([F:9])[c:10]([NH2:11])[cH:17]1.Cl[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]Cl>>[CH3:1][S:2](=[O:3])(=[O:4])[c:5]1[cH:6][cH:7][c:8]([F:9])[c:10]([N:11]2[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]2)[cH:17]1
CS(=O)(=O)c1ccc(F)c(N)c1.ClCCNCCCl
CS(=O)(=O)c1ccc(F)c(N2CCNCC2)c1
null
null
ClC1=C(C=CC=C1)Cl
Heteroatom Alkylation and Arylation
OtherReaction
dec7615731d236f383a5e0021b2ac4287f587bb876f98147d27e03daac7cbefb
631870b1ab33be0edc94bc9ae10321f1c5ede4dd4db77035c9d3979e4a2118fb
c1ccc(N2CCNCC2)cc1
Cl-[CH2;D2;+0:1]-[C:2]-[#7:3]-[C:4]-[CH2;D2;+0:5]-Cl.[NH2;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[c:8]:[c:7](-[N;H0;D3;+0:6]1-[CH2;D2;+0:1]-[C:2]-[#7:3]-[C:4]-[CH2;D2;+0:5]-1):[c:9]
39
[{"value": 39.0, "product": "FC1=C(C=C(C=C1)S(=O)(=O)C)N1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
10 mL solution of 432 mg 2-fluoro-5-methylsulfonylphenylamine (compound in Production Example 338) and 490 mg bis(2-chloroethyl)amine hydrochloride in 1,2-dichlorobenzene was stirred at 200° C. for 9 hours. The reaction mixture was neutralized by adding an aqueous saturated sodium bicarbonate solution and then extracte...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Primary amine
Tertiary amine
null
C1C[NH]CCN1
c1ccccc1.C1C[NH]CCN1
HCl
ClC1=C(C=CC=C1)Cl
null
null
CS(=O)(=O)c1ccc(F)c(N)c1.ClCCNCCCl>ClC1=C(C=CC=C1)Cl>CS(=O)(=O)c1ccc(F)c(N2CCNCC2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a7dcc9b3fced469691d85657b923039b
CC(C)(C)OC(=O)N1CCNCC1.N#Cc1cc(Br)ccc1F>>CC(C)(C)OC(=O)N1CCN(c2ccc(F)c(C#N)c2)CC1
C([O-])([O-])=O.[Cs+].[Cs+].BrC=1C=CC(=C(C#N)C1)F.N1(CCNCC1)C(=O)OC(C)(C)C.C1(=CC=CC=C1)P(C1=C(C2=CC=CC=C2C=C1)C1=C(C=CC2=CC=CC=C12)P(C1=CC=CC=C1)C1=CC=CC=C1)C1=CC=CC=C1>>C(#N)C=1C=C(C=CC1F)N1CCN(CC1)C(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][NH:11][CH2:21][CH2:22]1.Br[c:12]1[cH:13][cH:14][c:15]([F:16])[c:17]([C:18]#[N:19])[cH:20]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[cH:13][cH:14][c:15]([F:16])[c:17]([C:18]#[N:19])[cH:20]2)[CH2:21][CH2:22]1
CC(C)(C)OC(=O)N1CCNCC1.N#Cc1cc(Br)ccc1F
CC(C)(C)OC(=O)N1CCN(c2ccc(F)c(C#N)c2)CC1
null
[Pd].[Pd].C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1.C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1.C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
d687b31bdda9f407fdde6ca57e67eee0681e173646c617afef7770c56d05bab9
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc(N2CCNCC2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[#7:6]1-[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]-1>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:9]1-[C:10]-[C:11]-[#7:6]-[C:7]-[C:8]-1):[c:4]:[c:5]
null
[]
80
CELSIUS
10
MINUTE
1.24 g of 2,2′-bis (diphenylphosphino)-1,1′-binaphthyl and 229 mg of tris (dibenzylideneacetone) dipalladium were dissolved in toluene and stirred at 80° C. for 10 minutes. The reaction mixture was returned to room temperature, and 2.28 g cesium carbonate, 1.0 g 5-bromo-2-fluorobenzonitrile and 1.09 g t-butyl 1-piperaz...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1C[NH]CCN1.c1ccccc1
C1C[NH]CC[NH]1.c1ccccc1
C1C[NH]CC[NH]1.c1ccccc1
HBr
[Pd].[Pd].C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1.C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1.C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1.C1(=CC=CC=C1)C
80
0.166667
CC(C)(C)OC(=O)N1CCNCC1.N#Cc1cc(Br)ccc1F>[Pd].[Pd].C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1.C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1.C(C1=CC=CC=C1)=CC(=O)C=CC1=CC=CC=C1.C1(=CC=CC=C1)C>CC(C)(C)OC(=O)N1CCN(c2ccc(F)c(C#N)c2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f14653ef79f24d6b9ac4bda8f513752b
CC(C)(C)OC(=O)N1CCN(c2ccc(F)c(C#N)c2)CC1>>N#Cc1cc(N2CCNCC2)ccc1F
FC(C(=O)O)(F)F.C(#N)C=1C=C(C=CC1F)N1CCN(CC1)C(=O)OC(C)(C)C.O.N>>FC1=C(C#N)C=C(C=C1)N1CCNCC1
CC(C)(C)OC(=O)[N:9]1[CH2:8][CH2:7][N:6]([c:5]2[cH:4][c:3]([C:2]#[N:1])[c:14]([F:15])[cH:13][cH:12]2)[CH2:11][CH2:10]1>>[N:1]#[C:2][c:3]1[cH:4][c:5]([N:6]2[CH2:7][CH2:8][NH:9][CH2:10][CH2:11]2)[cH:12][cH:13][c:14]1[F:15]
CC(C)(C)OC(=O)N1CCN(c2ccc(F)c(C#N)c2)CC1
N#Cc1cc(N2CCNCC2)ccc1F
null
null
null
Reduction
Boc amine deprotection
2c25e19aee181a3c5131cfdfda27035fd54d4379a11d745dfb75d386bacfd500
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc(N2CCNCC2)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1>>[#7:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:6]-[C:5]-1
101.2
[{"value": 101.2, "product": "FC1=C(C#N)C=C(C=C1)N1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Trifluoroacetic acid was added to 500 mg of t-butyl 4-(3-cyano-4-fluorophenyl)-1-piperazinecarboxylate (compound in Production Example 354) and stirred at room temperature for several hours. After the reaction solution was cooled on ice, ammonia water was added thereto and stirred, the aqueous layer was extracted with ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1C[NH]CC[NH]1
C1C[NH]CCN1
c1ccccc1.C1C[NH]CCN1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCN(c2ccc(F)c(C#N)c2)CC1>>N#Cc1cc(N2CCNCC2)ccc1F
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dc435eadabab4c7aab992d48ebc7c27f
C1CNCCN1.CS(=O)(=O)c1ccc(Br)cc1>>CS(=O)(=O)c1ccc(N2CCNCC2)cc1
BrC1=CC=C(C=C1)S(=O)(=O)C.N1CCNCC1>>CS(=O)(=O)C1=CC=C(C=C1)N1CCNCC1
[NH:9]1[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]1.Br[c:8]1[cH:7][cH:6][c:5]([S:2]([CH3:1])(=[O:3])=[O:4])[cH:16][cH:15]1>>[CH3:1][S:2](=[O:3])(=[O:4])[c:5]1[cH:6][cH:7][c:8]([N:9]2[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]2)[cH:15][cH:16]1
C1CNCCN1.CS(=O)(=O)c1ccc(Br)cc1
CS(=O)(=O)c1ccc(N2CCNCC2)cc1
null
[I-].C(CCC)[N+](CCCC)(CCCC)CCCC
O
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
1d452876efa46787ecd5eab4acf018720843b51fbe40244616ffd72f6a602335
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc(N2CCNCC2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[#7:6]1-[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]-1>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:9]1-[C:8]-[C:7]-[#7:6]-[C:11]-[C:10]-1):[c:4]:[c:5]
91.3
[{"value": 91.3, "product": "CS(=O)(=O)C1=CC=C(C=C1)N1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
A mixture of 3.0 g 1-bromo-4-methylsulfonyl benzene, 3.3 g piperazine and 470 mg tetrabutyl ammonium iodide was stirred at 120° C. to 140° C. for 5 hours. Water was added to the mixture, then insolubles were filtered off, the filtrate was extracted with dichloromethane. The organic layer was washed with brine and dried...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CNCCN1.c1ccccc1
c1ccccc1.C1C[NH]CCN1
c1ccccc1.C1C[NH]CCN1
HBr
[I-].C(CCC)[N+](CCCC)(CCCC)CCCC.O
null
5
C1CNCCN1.CS(=O)(=O)c1ccc(Br)cc1>[I-].C(CCC)[N+](CCCC)(CCCC)CCCC.O>CS(=O)(=O)c1ccc(N2CCNCC2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2459a44217094dd5933f672c4625039f
Brc1ccc2ncnc(-c3cccs3)c2c1.O=S(=O)(O)Cl>>O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1
ClS(=O)(=O)O.S(=O)(Cl)Cl.BrC=1C=C2C(=NC=NC2=CC1)C=1SC=CC1>>BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)S(=O)(=O)Cl
[cH:5]1[cH:6][cH:7][c:8](-[c:9]2[n:10][cH:11][n:12][c:13]3[cH:14][cH:15][c:16]([Br:17])[cH:18][c:19]23)[s:20]1.O[S:2](=[O:1])(=[O:3])[Cl:4]>>[O:1]=[S:2](=[O:3])([Cl:4])[c:5]1[cH:6][cH:7][c:8](-[c:9]2[n:10][cH:11][n:12][c:13]3[cH:14][cH:15][c:16]([Br:17])[cH:18][c:19]23)[s:20]1
Brc1ccc2ncnc(-c3cccs3)c2c1.O=S(=O)(O)Cl
O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1
null
null
O
Heteroatom Alkylation and Arylation
Aromatic sulfonyl chlorination
8262cd7e2fb49c292864204e18c959a9ad65e1b79f29da3707f938430466ad5f
d32b60b8f9bfd187c6c9f1eef6a22a00f53525a7532b83aba763d5389c9e4280
c1csc(-c2ncnc3ccccc23)c1
O-[S;H0;D4;+0:1](-[Cl;D1;H0:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#16;a:5]1:[c:6]:[c:7]:[c:8]:[cH;D2;+0:9]:1>>[Cl;D1;H0:2]-[S;H0;D4;+0:1](=[O;D1;H0:3])(=[O;D1;H0:4])-[c;H0;D3;+0:9]1:[#16;a:5]:[c:6]:[c:7]:[c:8]:1
null
[]
60
CELSIUS
null
null
0.18 mL chlorosulfonic acid and 0.19 mL thionyl chloride were added to 0.1 g of 6-bromo-4-(2-thienyl)quinazoline (compound in Production Example 96) under ice-cooling in a stream of nitrogen, and the mixture was heated for 13 hours at 60° C., then neutralized by adding water and a sodium bicarbonate solution and extrac...
10.6084/m9.figshare.5104873.v1
null
null
Sulfonyl halide
c1ccsc1
c1ccsc1
c1ccsc1.c1ccc2ncncc2c1
HO-
O
60
null
Brc1ccc2ncnc(-c3cccs3)c2c1.O=S(=O)(O)Cl>O>O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2f60f7cf671249b0acf69f03ed62bc04
Brc1ccc2ncnc(-c3cccs3)c2c1.O=S(=O)(O)Cl>>O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1
C([O-])(O)=O.[Na+].ClS(=O)(=O)O.S(=O)(Cl)Cl.BrC=1C=C2C(=NC=NC2=CC1)C=1SC=CC1>>BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)S(=O)(=O)Cl
[cH:5]1[cH:6][cH:7][c:8](-[c:9]2[n:10][cH:11][n:12][c:13]3[cH:14][cH:15][c:16]([Br:17])[cH:18][c:19]23)[s:20]1.O=[S:2]([OH:1])(=[O:3])[Cl:4]>>[O:1]=[S:2](=[O:3])([Cl:4])[c:5]1[cH:6][cH:7][c:8](-[c:9]2[n:10][cH:11][n:12][c:13]3[cH:14][cH:15][c:16]([Br:17])[cH:18][c:19]23)[s:20]1
Brc1ccc2ncnc(-c3cccs3)c2c1.O=S(=O)(O)Cl
O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1
null
null
O
Protection
Aromatic sulfonyl chlorination
218ad6407b184db382d4e28de34d7ac34a86551588ce92c2c215481758bc8ff4
c731d053565135be022f3edbe36cf28a9b4364ca579bdb183b2db9578bab4695
c1csc(-c2ncnc3ccccc23)c1
O=[S;H0;D4;+0:1](-[Cl;D1;H0:2])(=[O;D1;H0:3])-[OH;D1;+0:4].[#16;a:5]1:[c:6]:[c:7]:[c:8]:[cH;D2;+0:9]:1>>[Cl;D1;H0:2]-[S;H0;D4;+0:1](=[O;D1;H0:3])(=[O;H0;D1;+0:4])-[c;H0;D3;+0:9]1:[#16;a:5]:[c:6]:[c:7]:[c:8]:1
null
[]
60
CELSIUS
null
null
14.4 mL chlorosulfonic acid and 14.42 mL thionyl chloride were added to 7.78 g of 6-bromo-4-(2-thienyl)quinazoline (compound in Production Example 96) under ice-cooling in a stream of nitrogen, and the mixture was heated at 60° C. for 16 hours, then poured into iced water, neutralized by adding a sodium bicarbonate sol...
10.6084/m9.figshare.5104873.v1
null
null
Sulfonyl halide
c1ccsc1
c1ccsc1
c1ccsc1.c1ccc2ncncc2c1
HO-
O
60
null
Brc1ccc2ncnc(-c3cccs3)c2c1.O=S(=O)(O)Cl>O>O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a7ce280c114f486cab7c929a87e21d54
CN.O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1>>CNS(=O)(=O)c1ccc(-c2ncnc3ccc(Br)cc23)s1
BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)S(=O)(=O)Cl.CN>>CNS(=O)(=O)C=1SC(=CC1)C1=NC=NC2=CC=C(C=C12)Br
[CH3:1][NH2:2].Cl[S:3](=[O:4])(=[O:5])[c:6]1[cH:7][cH:8][c:9](-[c:10]2[n:11][cH:12][n:13][c:14]3[cH:15][cH:16][c:17]([Br:18])[cH:19][c:20]23)[s:21]1>>[CH3:1][NH:2][S:3](=[O:4])(=[O:5])[c:6]1[cH:7][cH:8][c:9](-[c:10]2[n:11][cH:12][n:13][c:14]3[cH:15][cH:16][c:17]([Br:18])[cH:19][c:20]23)[s:21]1
CN.O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1
CNS(=O)(=O)c1ccc(-c2ncnc3ccc(Br)cc23)s1
null
null
O1CCCC1
Miscellaneous
Sulfonamide synthesis (Schotten-Baumann) primary amine
a86b0632821e188c0a5dc5a5a2aac298ab3eccaee8a52ba46078c3d5975a290d
50f8fbf3d327483c3eeff8f6cbd4065e4c7600bb501fbe08958a5c79a0926428
c1csc(-c2ncnc3ccccc23)c1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[#16;a:6]:[c:7].[C;D1;H3:8]-[NH2;D1;+0:9]>>[C;D1;H3:8]-[NH;D2;+0:9]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[#16;a:6]:[c:7]
null
[]
null
null
1
HOUR
800 mg of 5-(6-bromoquinazolin-4-yl)-thiophen-2-sulfonyl chloride (compound in Production Example 377) was dissolved in 15 mL tetrahydrofuran, and 1.78 mL methylamine was added thereto and stirred at room temperature for 1 hour. The solvent was removed, and the residue was purified by silica gel column chromatography (...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccsc1.c1ccc2ncncc2c1
HCl
O1CCCC1
null
1
CN.O=S(=O)(Cl)c1ccc(-c2ncnc3ccc(Br)cc23)s1>O1CCCC1>CNS(=O)(=O)c1ccc(-c2ncnc3ccc(Br)cc23)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6519ac15518343e7928c1bc845e13259
CCOC(OCC)c1ccc(-c2ncnc3ccc(Br)cc23)s1>>O=Cc1ccc(-c2ncnc3ccc(Br)cc23)s1
BrC=1C=C2C(=NC=NC2=CC1)C=1SC(=CC1)C(OCC)OCC.FC(C(=O)O)(F)F.O>>BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)C=O
CCO[CH:2]([O:1]CC)[c:3]1[cH:4][cH:5][c:6](-[c:7]2[n:8][cH:9][n:10][c:11]3[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]23)[s:18]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[n:8][cH:9][n:10][c:11]3[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]23)[s:18]1
CCOC(OCC)c1ccc(-c2ncnc3ccc(Br)cc23)s1
O=Cc1ccc(-c2ncnc3ccc(Br)cc23)s1
null
null
ClCCl
Miscellaneous
Acetal hydrolysis to aldehyde
2c5baf4818f438d514702dbb9f9a64f069b67040aebce8bef29fab8232955599
84d5a69453aa750f462aa94a6bf2116fc17c5d88a9619aaa9eefb74b0c09848d
c1csc(-c2ncnc3ccccc23)c1
C-C-O-[CH;D3;+0:1](-[O;H0;D2;+0:2]-C-C)-[c:3](:[c:4]):[#16;a:5]:[c:6]>>[O;H0;D1;+0:2]=[CH;D2;+0:1]-[c:3](:[c:4]):[#16;a:5]:[c:6]
98.1
[{"value": 98.1, "product": "BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
2.6 g of 6-bromo-4-(5-diethoxymethylthiophen-2-yl)quinazoline (compound in Production Example 380) was dissolved in 10 mL dichloromethane, then 5 mL trifluoroacetic acid was added thereto, and the mixture was stirred at room temperature for 3 hours, neutralized by adding water and a sodium bicarbonate solution, and ext...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Aldehyde
null
null
c1ccsc1.c1ccc2ncncc2c1
HO-
ClCCl
null
3
CCOC(OCC)c1ccc(-c2ncnc3ccc(Br)cc23)s1>ClCCl>O=Cc1ccc(-c2ncnc3ccc(Br)cc23)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9130d476b2234cf9a01bb669ea3c511b
O=Cc1ccc(-c2ncnc3ccc(Br)cc23)s1.[OH-]>>O=C(O)c1ccc(-c2ncnc3ccc(Br)cc23)s1
BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)C=O.[OH-].[Na+]>>BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)C(=O)O
[O:1]=[CH:2][c:4]1[cH:5][cH:6][c:7](-[c:8]2[n:9][cH:10][n:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][c:18]23)[s:19]1.[OH-:3]>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7](-[c:8]2[n:9][cH:10][n:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][c:18]23)[s:19]1
O=Cc1ccc(-c2ncnc3ccc(Br)cc23)s1.[OH-]
O=C(O)c1ccc(-c2ncnc3ccc(Br)cc23)s1
null
[N+](=O)([O-])[O-].[Ag+]
O.CS(=O)C
Acylation
OtherReaction
212580cf94343ba681451fe636f6c4d850d6e10e1bdc7e1852b33ddb4cd6898f
37c4d4a9954dede23d940a212db876610ae18deb2faf143c8b44e17692b9193f
c1csc(-c2ncnc3ccccc23)c1
[O;D1;H0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[#16;a:5]:[c:6].[OH-;D0:7]>>[O;D1;H0:1]=[C;H0;D3;+0:2](-[OH;D1;+0:7])-[c:3](:[c:4]):[#16;a:5]:[c:6]
82.6
[{"value": 82.6, "product": "BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)C(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution of 2.19 g silver nitrate in 40 mL water and a solution of 1.96 g 5-(6-bromoquinazolin-4-yl)thiophen-2-carboaldehyde (compound in Production Example 381) in 20 mL dimethyl sulfoxide were added little by little successively to a solution of 1.0 g sodium hydroxide in 40 mL water under ice-cooling, and the mixtu...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Carboxylic acid
null
null
c1ccsc1.c1ccc2ncncc2c1
null
[N+](=O)([O-])[O-].[Ag+].O.CS(=O)C
null
24
O=Cc1ccc(-c2ncnc3ccc(Br)cc23)s1.[OH-]>[N+](=O)([O-])[O-].[Ag+].O.CS(=O)C>O=C(O)c1ccc(-c2ncnc3ccc(Br)cc23)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a33f2b4bd31c4863a209666470456a1f
Nc1ccc(F)cc1F.O=C(O)c1ccc(-c2ncnc3ccc(Br)cc23)s1>>O=C(Nc1ccc(F)cc1F)c1ccc(-c2ncnc3ccc(Br)cc23)s1
C(C)N(CC)CC.C(OCC(C)C)(=O)Cl.BrC=1C=C2C(=NC=NC2=CC1)C1=CC=C(S1)C(=O)O.FC1=C(C=CC(=C1)F)N>>FC1=C(C=CC(=C1)F)NC(=O)C=1SC(=CC1)C1=NC=NC2=CC=C(C=C12)Br
[NH2:3][c:4]1[cH:5][cH:6][c:7]([F:8])[cH:9][c:10]1[F:11].O[C:2](=[O:1])[c:12]1[cH:13][cH:14][c:15](-[c:16]2[n:17][cH:18][n:19][c:20]3[cH:21][cH:22][c:23]([Br:24])[cH:25][c:26]23)[s:27]1>>[O:1]=[C:2]([NH:3][c:4]1[cH:5][cH:6][c:7]([F:8])[cH:9][c:10]1[F:11])[c:12]1[cH:13][cH:14][c:15](-[c:16]2[n:17][cH:18][n:19][c:20]3[cH...
Nc1ccc(F)cc1F.O=C(O)c1ccc(-c2ncnc3ccc(Br)cc23)s1
O=C(Nc1ccc(F)cc1F)c1ccc(-c2ncnc3ccc(Br)cc23)s1
null
null
O1CCCC1.O
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(Nc1ccccc1)c1ccc(-c2ncnc3ccccc23)s1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#16;a:5]:[c:6].[NH2;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10])-[c:3](:[c:4]):[#16;a:5]:[c:6]
42.8
[{"value": 42.8, "product": "FC1=C(C=CC(=C1)F)NC(=O)C=1SC(=CC1)C1=NC=NC2=CC=C(C=C12)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
300 mg of 5-(6-bromoquinazolin-4-yl)thiophen-2-carboxylic acid (compound in Production Example 382) was dissolved in 4 mL tetrahydrofuran, then 0.37 mL triethylamine and 0.14 mL isobutyl chlorocarbonate were added thereto under ice-cooling, and the mixture was stirred for 1 hour under nitrogen atmosphere. This mixture ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccsc1.c1ccc2ncncc2c1
HO-
O1CCCC1.O
null
1
Nc1ccc(F)cc1F.O=C(O)c1ccc(-c2ncnc3ccc(Br)cc23)s1>O1CCCC1.O>O=C(Nc1ccc(F)cc1F)c1ccc(-c2ncnc3ccc(Br)cc23)s1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6166f5ee7a5447d7a41b08353050cb49
NC1CC1.O=C(O)c1ccc(-c2ncnc3ccc(Cl)cc23)cc1F>>O=C(NC1CC1)c1ccc(-c2ncnc3ccc(Cl)cc23)cc1F
F[P-](F)(F)(F)(F)F.N1(N=NC2=C1C=CC=C2)O[P+](N(C)C)(N(C)C)N(C)C.ClC=1C=C2C(=NC=NC2=CC1)C1=CC(=C(C(=O)O)C=C1)F.C1(CC1)N.C(C)N(CC)CC>>ClC=1C=C2C(=NC=NC2=CC1)C1=CC(=C(C(=O)NC2CC2)C=C1)F
[NH2:3][CH:4]1[CH2:5][CH2:6]1.O[C:2](=[O:1])[c:7]1[cH:8][cH:9][c:10](-[c:11]2[n:12][cH:13][n:14][c:15]3[cH:16][cH:17][c:18]([Cl:19])[cH:20][c:21]23)[cH:22][c:23]1[F:24]>>[O:1]=[C:2]([NH:3][CH:4]1[CH2:5][CH2:6]1)[c:7]1[cH:8][cH:9][c:10](-[c:11]2[n:12][cH:13][n:14][c:15]3[cH:16][cH:17][c:18]([Cl:19])[cH:20][c:21]23)[cH:2...
NC1CC1.O=C(O)c1ccc(-c2ncnc3ccc(Cl)cc23)cc1F
O=C(NC1CC1)c1ccc(-c2ncnc3ccc(Cl)cc23)cc1F
null
null
ClCCl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(NC1CC1)c1ccc(-c2ncnc3ccccc23)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[NH2;D1;+0:6]-[C:7]1-[C:8]-[C:9]-1>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[NH;D2;+0:6]-[C:7]1-[C:8]-[C:9]-1)-[c:3](:[c:4]):[c:5]
71.7
[{"value": 71.7, "product": "ClC=1C=C2C(=NC=NC2=CC1)C1=CC(=C(C(=O)NC2CC2)C=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
0.2 g 4-(6-chloroquinazolin-4-yl)-2-fluorobenzoic acid (compound in Production Example 386), 41 mg cyclopropylamine and 0.12 mL triethylamine were dissolved in 6 mL dichloromethane, then 320 mg benzotriazol-1-yloxytris(dimethylamino)-phosphonium hexafluorophosphate was added thereto, and the mixture was stirred at room...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
C1CC1.c1ccccc1.c1ccc2ncncc2c1
HO-
ClCCl
null
3
NC1CC1.O=C(O)c1ccc(-c2ncnc3ccc(Cl)cc23)cc1F>ClCCl>O=C(NC1CC1)c1ccc(-c2ncnc3ccc(Cl)cc23)cc1F