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-0387783899c642a8b7eb4ba379bcdf5d
ord-c220962fb2bf497885276694ceb1098c
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1.CCO>>Oc1nccc2c(NC3CCNCC3)cccc12
ClC1=NC=CC2=C(C=CC=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.C(C)O>>Cl.OC1=NC=CC2=C(C=CC=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:13]1[CH2:12][CH2:11][CH:10]([NH:9][c:8]2[c:7]3[cH:6][cH:5][n:4][c:3](Cl)[c:19]3[cH:18][cH:17][cH:16]2)[CH2:15][CH2:14]1.CC[OH:2]>>[OH:2][c:3]1[n:4][cH:5][cH:6][c:7]2[c:8]([NH:9][CH:10]3[CH2:11][CH2:12][NH:13][CH2:14][CH2:15]3)[cH:16][cH:17][cH:18][c:19]12
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1.CCO
Oc1nccc2c(NC3CCNCC3)cccc12
null
null
C(C)OCC
Heteroatom Alkylation and Arylation
OtherReaction
4be42df42161d3e4501211268c062b45b3d4e25d60ed59a2658de168f9194226
de2f28cc1c3a2a95cdd3d1ada4dc87abcced8bfbcdb89c7e6652b9ee92c9e650
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5].Cl-[c;H0;D3;+0:6](:[#7;a:7]:[c:8]):[c:9](:[c:10]):[c:11].C-C-[OH;D1;+0:12]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5].[OH;D1;+0:12]-[c;H0;D3;+0:6](:[#7;a:7]:[c:8]):[c:9](:[c:10]):[c:11]
null
[]
85
CELSIUS
null
null
Intermediate 84 (76.6 mg) was added with concentrated hydrochloric acid (1.5 ml) and stirred with heating at 85° C. for 7 hours. The reaction mixture was cooled to room temperature, and then the residue was added with ethanol (1 ml) and diethyl ether (2 ml). The deposited precipitates were collected by filtration and w...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ether.Primary alcohol.Boc
Aromatic alcohol.Secondary amine
C1CC[NH]CC1.c1ccc2cnccc2c1
C1CCNCC1.c1ccc2cnccc2c1
C1CCNCC1.c1ccc2cnccc2c1
HCl
C(C)OCC
85
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1.CCO>C(C)OCC>Oc1nccc2c(NC3CCNCC3)cccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-46e100f7ec384b35afcd5adf91303a2d
C=Cc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12>>C=Cc1cncc2cccc(NC3CCC(N)CC3)c12
C(C)(C)(C)OC(=O)NC1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)C=C.Cl.CO>>Cl.C(=C)C1=CN=CC2=CC=CC(=C12)NC1CCC(CC1)N
CC(C)(C)OC(=O)[NH:17][CH:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([CH:2]=[CH2:1])[c:20]32)[CH2:19][CH2:18]1>>[CH2:1]=[CH:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][CH:16]([NH2:17])[CH2:18][CH2:19]3)[c:20]12
C=Cc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12
C=Cc1cncc2cccc(NC3CCC(N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 85 (85.5 mg) and 10% hydrogen chloride/methanol solution (2 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
C=Cc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12>>C=Cc1cncc2cccc(NC3CCC(N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c94c7c5195254876a3b661a5dd0755df
CCc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12>>CCc1cncc2cccc(NC3CCC(N)CC3)c12
C(C)(C)(C)OC(=O)NC1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)CC.Cl.CO>>Cl.C(C)C1=CN=CC2=CC=CC(=C12)NC1CCC(CC1)N
CC(C)(C)OC(=O)[NH:17][CH:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([CH2:2][CH3:1])[c:20]32)[CH2:19][CH2:18]1>>[CH3:1][CH2:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][CH:16]([NH2:17])[CH2:18][CH2:19]3)[c:20]12
CCc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12
CCc1cncc2cccc(NC3CCC(N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 86 (133 mg) and 10% hydrogen chloride/methanol solution (2 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
CCc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12>>CCc1cncc2cccc(NC3CCC(N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5ea2cb1dd9a846b5bf3301835d03cccb
Brc1cncc2ccccc12.N>>Nc1cncc2ccccc12
BrC1=CN=CC2=CC=CC=C12.N>>NC1=CN=CC2=CC=CC=C12
Br[c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]12.[NH3:1]>>[NH2:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]12
Brc1cncc2ccccc12.N
Nc1cncc2ccccc12
null
O.O.O.O.O.S(=O)(=O)([O-])[O-].[Cu+2]
O1CCOCC1
Heteroatom Alkylation and Arylation
OtherReaction
261fd9f972974897261ca5eac8b1086caae005655bedee979c411e5b22857ba2
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1ccc2cnccc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7].[NH3;D0;+0:8]>>[NH2;D1;+0:8]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
null
[]
165
CELSIUS
21
HOUR
A suspension of 4-bromoisoquinoline (25.0 g), copper(II) sulfate pentahydrate (30.4 g, Nacalai Tesque), 28% aqueous ammonia (100 ml) and 1,4-dioxane (100 ml) was stirred in a sealed tube at 165° C. for 21 hours. The reaction mixture was cooled to room temperature, the insoluble matters were removed by filtration throug...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HBr
O.O.O.O.O.S(=O)(=O)([O-])[O-].[Cu+2].O1CCOCC1
165
21
Brc1cncc2ccccc12.N>O.O.O.O.O.S(=O)(=O)([O-])[O-].[Cu+2].O1CCOCC1>Nc1cncc2ccccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6e55001f2da4432ebe9991fc4a77c3aa
Cl.Nc1cncc2ccccc12>>Clc1cncc2ccccc12
Cl.NC1=CN=CC2=CC=CC=C12.Cl.N(=O)[O-].[Na+].N>>ClC1=CN=CC2=CC=CC=C12
[ClH:1].N[c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]12>>[Cl:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]12
Cl.Nc1cncc2ccccc12
Clc1cncc2ccccc12
null
[Cu]Cl
null
Miscellaneous
OtherReaction
a80b46bfc720178a7247f763a2a5c279a0921fee09e9f9f15b3416ca42dac62e
1129c10513c603d2647e51dd9713063aaf10bd8a364ed275b9b93c32624e3ba4
c1ccc2cnccc2c1
N-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7].[ClH;D0;+0:8]>>[Cl;H0;D1;+0:8]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
null
[]
null
null
15
HOUR
Intermediate 87 (1.27 g) was dissolved in 1 N aqueous hydrochloric acid (36 ml) and added dropwise with an aqueous solution (36 ml) of sodium nitrite (1.21 g, Wako Pure Chemical Industries) with ice cooling. The obtained suspension was added dropwise to a solution of copper(I) chloride (1.83 g, Wako Pure Chemical Indus...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Aromatic halide
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
Other
[Cu]Cl
null
15
Cl.Nc1cncc2ccccc12>[Cu]Cl>Clc1cncc2ccccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d8ae3de07dce41eb80afac012049edb2
Clc1cncc2ccccc12>>O=[N+]([O-])c1cccc2cncc(Cl)c12
ClC1=CN=CC2=CC=CC=C12.[N+](=O)([O-])[O-].[K+].N>>ClC1=CN=CC2=CC=CC(=C12)[N+](=O)[O-]
[cH:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][c:12]([Cl:13])[c:14]12>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][c:12]([Cl:13])[c:14]12
Clc1cncc2ccccc12
O=[N+]([O-])c1cccc2cncc(Cl)c12
null
null
S(O)(O)(=O)=O
Functional Group Addition
OtherReaction
af041d80e34a3ce46b5eb910f230615587e5ab9eb4305ac845f1ae2dbd577a25
22f3183026a2d99c91ec0c53f0059a15c8421016bd62c8ab45281362b96dc686
c1ccc2cnccc2c1
[c:1]:[c:2]:[cH;D2;+0:3]:[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1>>[O;-;D1;H0:10]-[#7;+:11](=[O;D1;H0:12])-[c;H0;D3;+0:3](:[c:2]:[c:1]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
69.4
[{"value": 69.4, "product": "ClC1=CN=CC2=CC=CC(=C12)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
Intermediate 88 (375 mg) was dissolved in concentrated sulfuric acid (2 ml), then added with potassium nitrate (260 mg) with ice cooling and stirred for 2 hours. The reaction mixture was added with 28% aqueous ammonia (10 ml) and extracted twice with ethyl acetate (15 ml for each time). The organic layer was dried over...
10.6084/m9.figshare.5104873.v1
null
null
Nitro group
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
Other
S(O)(O)(=O)=O
null
2
Clc1cncc2ccccc12>S(O)(O)(=O)=O>O=[N+]([O-])c1cccc2cncc(Cl)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fcdc390576094c1d8a9ce9abd10a933f
O=[N+]([O-])c1cccc2cncc(Cl)c12>>Nc1cccc2cncc(Cl)c12
O.O.[Sn](Cl)Cl.ClC1=CN=CC2=CC=CC(=C12)[N+](=O)[O-].[OH-].[Na+]>>ClC1=CN=CC2=CC=CC(=C12)N
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][n:8][cH:9][c:10]([Cl:11])[c:12]12>>[NH2:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][n:8][cH:9][c:10]([Cl:11])[c:12]12
O=[N+]([O-])c1cccc2cncc(Cl)c12
Nc1cccc2cncc(Cl)c12
null
null
Cl
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2cnccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
67.5
[{"value": 67.5, "product": "ClC1=CN=CC2=CC=CC(=C12)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Tin(II) chloride dihydrate (1.70 g) was dissolved in concentrated hydrochloric acid (1 ml), added with a mixture of Intermediate 89 (315 mg) and 2 N aqueous hydrochloric acid (2 ml) with ice cooling and refluxed with heating for 2 hours. The reaction mixture was cooled to room temperature, added with 5 N aqueous sodium...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2cnccc2c1
Other
Cl
null
null
O=[N+]([O-])c1cccc2cncc(Cl)c12>Cl>Nc1cccc2cncc(Cl)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-72438e154c334ea6b03363a7903a683d
CC(C)(C)OC(=O)N1CCC(=O)CC1.Nc1cccc2cncc(Cl)c12>>CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Cl)c23)CC1
C(O)([O-])=O.[Na+].ClC1=CN=CC2=CC=CC(=C12)N.O=C1CCN(CC1)C(=O)OC(C)(C)C.[BH4-].[Na+]>>ClC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C
O=[C:11]1[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:25][CH2:24]1.[NH2:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[cH:18][n:19][cH:20][c:21]([Cl:22])[c:23]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([NH:12][c:13]2[cH:14][cH:15][cH:16][c:17]3[cH:18][n:19][cH...
CC(C)(C)OC(=O)N1CCC(=O)CC1.Nc1cccc2cncc(Cl)c12
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Cl)c23)CC1
null
CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4]
CO.ClCCl
Heteroatom Alkylation and Arylation
Reductive amination with ketone
42e9e55fb09951ae64da272b20a0fe6708e6155493933c6a5b57bd203fbe3626
07faf85ffe990e88a1de7fd04a339bf226f78d8bfae9712ea59eebd76bb54b9f
c1cc(NC2CCNCC2)c2ccncc2c1
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1.[NH2;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[c:9]:[c:8](-[NH;D2;+0:7]-[CH;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1):[c:10]
21.8
[{"value": 21.8, "product": "ClC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
138
HOUR
According to the method of Example 103, Step A, a mixture of Intermediate 90 (121 mg), tert-butyl 4-oxo-1-piperidinecarboxylate (274 mg), titanium tetraisopropoxide (0.41 ml) and dichloromethane (7 ml) was stirred at room temperature for 138 hours. The reaction mixture was added with sodium borohydride (114 mg) and met...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
Secondary amine
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccc2cnccc2c1
Other
CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4].CO.ClCCl
null
138
CC(C)(C)OC(=O)N1CCC(=O)CC1.Nc1cccc2cncc(Cl)c12>CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4].CO.ClCCl>CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Cl)c23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-caa7bc7c670f452e8af4aeec035bb7bb
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Cl)c23)CC1>>Clc1cncc2cccc(NC3CCNCC3)c12
ClC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.ClC1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([Cl:2])[c:19]32)[CH2:18][CH2:17]1>>[Cl:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)[c:19]12
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Cl)c23)CC1
Clc1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
230.4
[{"value": 230.4, "product": "Cl.ClC1=CN=CC2=CC=CC(=C12)NC1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 91 (53.5 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (1 ml) and diethyl ether (3 ml). The depo...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Cl)c23)CC1>>Clc1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2183330ad69d4daf8b0bf3debc9cee84
CC(C)(C)OC(=O)C1(N)CCC(=O)CC1.Nc1cccc2cncc(Cl)c12>>CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Cl)c23)CC1
C(O)([O-])=O.[Na+].ClC1=CN=CC2=CC=CC(=C12)N.O=C1CCC(CC1)(N)C(=O)OC(C)(C)C.[BH4-].[Na+]>>C(C)(C)(C)OC(=O)NC1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)Cl
O=[C:12]1[CH2:11][CH2:10][C:9]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])([NH2:8])[CH2:26][CH2:25]1.[NH2:13][c:14]1[cH:15][cH:16][cH:17][c:18]2[cH:19][n:20][cH:21][c:22]([Cl:23])[c:24]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH:9]1[CH2:10][CH2:11][CH:12]([NH:13][c:14]2[cH:15][cH:16][cH:17][c:18...
CC(C)(C)OC(=O)C1(N)CCC(=O)CC1.Nc1cccc2cncc(Cl)c12
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Cl)c23)CC1
null
CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4]
CO.ClCCl
Protection
OtherReaction
4a8cf36cfc07554ec0fcb4db795ad7e23fdcb78b4b4aa84e4f6291e0179bfb3f
156ca1cd24e8fdcd7296a675bc0ef4e78771844949b27717ab0d615ffde695c2
c1cc(NC2CCCCC2)c2ccncc2c1
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[C;H0;D4;+0:4](-[NH2;D1;+0:5])(-[C;H0;D3;+0:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12])-[C:13]-[C:14]-1.[NH2;D1;+0:15]-[c:16](:[c:17]):[c:18]>>[C;D1;H3:10]-[C:9](-[C;D1;H3:11])(-[C;D1;H3:12])-[#8:8]-[C;H0;D3;+0:6](=[O;D1;H0:7])-[NH;D2;+0:5]-[CH;D3;+0:4]1-[C:3]...
null
[]
null
null
120
HOUR
According to the method of Example 103, Step A, a mixture of Intermediate 90 (100 mg), tert-butyl 4-oxo-1-aminocyclohexylcarboxylate (270 mg), titanium tetraisopropoxide (0.34 ml) and dichloromethane (7 ml) was stirred at room temperature for 120 hours. The reaction mixture was added with sodium borohydride (94 mg) and...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Primary amine.Primary amine
Carbamic ester.Ether.Secondary amine.Boc
C1CCCCC1
C1CCCCC1
C1CCCCC1.c1ccc2cnccc2c1
Other
CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4].CO.ClCCl
null
120
CC(C)(C)OC(=O)C1(N)CCC(=O)CC1.Nc1cccc2cncc(Cl)c12>CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4].CO.ClCCl>CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Cl)c23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fd0fe1d1c92e49348e550fdf4bdb608e
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Cl)c23)CC1>>NC1CCC(Nc2cccc3cncc(Cl)c23)CC1
C(C)(C)(C)OC(=O)NC1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)Cl.Cl.CO>>Cl.ClC1=CN=CC2=CC=CC(=C12)NC1CCC(CC1)N
CC(C)(C)OC(=O)[NH:2][CH:3]1[CH2:4][CH2:5][CH:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][c:16]([Cl:17])[c:18]23)[CH2:19][CH2:20]1>>[NH2:2][CH:3]1[CH2:4][CH2:5][CH:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][c:16]([Cl:17])[c:18]23)[CH2:19][CH2:20]1
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Cl)c23)CC1
NC1CCC(Nc2cccc3cncc(Cl)c23)CC1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
225.3
[{"value": 225.3, "product": "Cl.ClC1=CN=CC2=CC=CC(=C12)NC1CCC(CC1)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 92 (40.4 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (1 ml) and diethyl ether (3 ml). The depo...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Cl)c23)CC1>>NC1CCC(Nc2cccc3cncc(Cl)c23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4b5eef1a0b364453826833678fecada6
Cc1cncc2ccccc12.O=C1CCC(=O)N1Br>>Cc1cncc2cccc(Br)c12
CC1=CN=CC2=CC=CC=C12.BrN1C(CCC1=O)=O.N>>BrC1=C2C(=CN=CC2=CC=C1)C
[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:12]12.O=C1CCC(=O)N1[Br:11]>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([Br:11])[c:12]12
Cc1cncc2ccccc12.O=C1CCC(=O)N1Br
Cc1cncc2cccc(Br)c12
null
null
S(O)(O)(=O)=O
Functional Group Interconversion
Bromination
9cac9f3adaa01c5b3ba77ecc78b3325ca368823796a491b3ff1d81b1acdc724d
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccc2cnccc2c1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[c:2]:[c:3]:[cH;D2;+0:4]:[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:4](:[c:3]:[c:2]):[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1
null
[]
null
null
2
HOUR
4-Methylisoquinoline (0.1 ml, synthesized according to the method described in Tetrahedron. Lett. 34, 45, 7239 (1993)) was dissolved in concentrated sulfuric acid (1 ml), then added with N-bromosuccinimide (125 mg) with ice cooling and stirred for 2 hours. The reaction mixture was added with 28% aqueous ammonia (5 ml) ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1ccc2cnccc2c1.C1CCNC1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HO-
S(O)(O)(=O)=O
null
2
Cc1cncc2ccccc12.O=C1CCC(=O)N1Br>S(O)(O)(=O)=O>Cc1cncc2cccc(Br)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2ef5bc5c67c04ed392a15b43bd1a3710
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1.Cc1cncc2cccc(Br)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@H](NC(=O)OC(C)(C)C)CC3)c12
BrC1=C2C(=CN=CC2=CC=C1)C.BrC1=C2C(=CN=CC2=CC=C1)C.C(C)(C)(C)P(C(C)(C)C)C(C)(C)C.C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)N.CC(C)([O-])C.[Na+]>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)NC1=C2C(=CN=CC2=CC=C1)C
[NH2:11][C@@H:12]1[CH2:13][CH2:14][C@H:15]([NH:16][C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[CH2:24][CH2:25]1.Br[c:10]1[cH:9][cH:8][cH:7][c:6]2[cH:5][n:4][cH:3][c:2]([CH3:1])[c:26]21>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][C@H:12]3[CH2:13][CH2:14][C@@H:15]([NH:16][C:17](=[O:1...
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1.Cc1cncc2cccc(Br)c12
Cc1cncc2cccc(N[C@@H]3CC[C@H](NC(=O)OC(C)(C)C)CC3)c12
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]
C(C)(=O)OCC.C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
17c3dbb58f19c559a89452c2c52a32d81319b5dd6d11e225611cc478eba61c1b
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1cc(NC2CCCCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[C:10]-[C:11](-[NH2;D1;+0:12])-[C:13]>>[C:10]-[C:11](-[NH;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1)-[C:13]
null
[]
120
CELSIUS
null
null
According to the method of Example 15, Step A, the title compound was synthesized from Intermediate 93. That is, under nitrogen atmosphere, a suspension of Intermediate 93 (602 mg), tris(dibenzylideneacetone)dipalladium(0) (124 mg), tri(tert-butyl)phosphine (0.5 ml, Kanto Chemicals), cis-N-(tert-butoxycarbonyl)-1,4-cyc...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1.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].C(C)(=O)OCC.C1(=CC=CC=C1)C
120
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1.Cc1cncc2cccc(Br)c12>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].C(C)(=O)OCC.C1(=CC=CC=C1)C>Cc1cncc2cccc(N[C@@H]3CC[C@H](NC(=O)OC(C)(C)C)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7592618e4e1244caaa2a448a9711696a
Cc1cncc2cccc(N[C@@H]3CC[C@H](NC(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@H](N)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)NC1=C2C(=CN=CC2=CC=C1)C.Cl.CO>>Cl.CC1=CN=CC2=CC=CC(=C12)N[C@@H]1CC[C@@H](CC1)N
CC(C)(C)OC(=O)[NH:16][C@@H:15]1[CH2:14][CH2:13][C@H:12]([NH:11][c:10]2[cH:9][cH:8][cH:7][c:6]3[cH:5][n:4][cH:3][c:2]([CH3:1])[c:19]32)[CH2:18][CH2:17]1>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][C@H:12]3[CH2:13][CH2:14][C@@H:15]([NH2:16])[CH2:17][CH2:18]3)[c:19]12
Cc1cncc2cccc(N[C@@H]3CC[C@H](NC(=O)OC(C)(C)C)CC3)c12
Cc1cncc2cccc(N[C@@H]3CC[C@H](N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 94 (35.8 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml). The ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
Cc1cncc2cccc(N[C@@H]3CC[C@H](NC(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@H](N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7a0d394d3d824ca4a3524777a3aa12a3
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](N)CC1.Cc1cncc2cccc(Br)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
BrC1=C2C(=CN=CC2=CC=C1)C.BrC1=C2C(=CN=CC2=CC=C1)C.C(C)(C)(C)P(C(C)(C)C)C(C)(C)C.C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)N.CC(C)([O-])C.[Na+]>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)NC1=C2C(=CN=CC2=CC=C1)C
[NH2:11][C@H:12]1[CH2:13][CH2:14][C@H:15]([NH:16][C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[CH2:24][CH2:25]1.Br[c:10]1[cH:9][cH:8][cH:7][c:6]2[cH:5][n:4][cH:3][c:2]([CH3:1])[c:26]21>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][C@H:12]3[CH2:13][CH2:14][C@H:15]([NH:16][C:17](=[O:18]...
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](N)CC1.Cc1cncc2cccc(Br)c12
Cc1cncc2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
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]
C(C)(=O)OCC.C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
17c3dbb58f19c559a89452c2c52a32d81319b5dd6d11e225611cc478eba61c1b
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1cc(NC2CCCCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[C:10]-[C:11](-[NH2;D1;+0:12])-[C:13]>>[C:10]-[C:11](-[NH;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1)-[C:13]
null
[]
120
CELSIUS
null
null
According to the method of Example 15, Step A, the title compound was synthesized from Intermediate 93. That is, under nitrogen atmosphere, a suspension of Intermediate 93 (1.13 g), tris(dibenzylideneacetone)dipalladium(0) (0.71 g), tri(tert-butyl)phosphine (0.5 ml), trans-N-(tert-butoxycarbonyl)-1,4-cyclohexanediamine...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1.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].C(C)(=O)OCC.C1(=CC=CC=C1)C
120
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](N)CC1.Cc1cncc2cccc(Br)c12>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].C(C)(=O)OCC.C1(=CC=CC=C1)C>Cc1cncc2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-59ed023d969d467280c5a315d794f41e
Cc1cncc2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@@H](N)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)NC1=C2C(=CN=CC2=CC=C1)C.Cl.CO>>Cl.CC1=CN=CC2=CC=CC(=C12)N[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:16][C@H:15]1[CH2:14][CH2:13][C@H:12]([NH:11][c:10]2[cH:9][cH:8][cH:7][c:6]3[cH:5][n:4][cH:3][c:2]([CH3:1])[c:19]32)[CH2:18][CH2:17]1>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][C@H:12]3[CH2:13][CH2:14][C@H:15]([NH2:16])[CH2:17][CH2:18]3)[c:19]12
Cc1cncc2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
Cc1cncc2cccc(N[C@@H]3CC[C@@H](N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 95 (389 mg) and 10% hydrogen chloride/methanol solution (10 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (2 ml) and diethyl ether (6 ml). The depo...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
Cc1cncc2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@@H](N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e66b85a64f8c49938e94e99c298be080
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.C[O-]>>COc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
BrC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.C[O-].[Na+].O>>COC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C
Br[c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][N:16]([C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[CH2:24][CH2:25]3)[c:26]12.[CH3:1][O-:2]>>[CH3:1][O:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][N:16]([C:17](=[O:18])[O:19][...
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.C[O-]
COc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
null
[Cu]I
CO.N1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
0f34e313d7c41dee60bf5f543b4ffe47bf78172f8b5a6c756b1c69b3aaf76dfb
51fd03eb6a688046e417b9ed09ea0e72062396d005af1318b9b5f376a97da959
c1cc(NC2CCNCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7].[C;D1;H3:8]-[O-;H0;D1:9]>>[C;D1;H3:8]-[O;H0;D2;+0:9]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
null
[]
65
CELSIUS
null
null
A suspension of Intermediate 71 (600 mg) and copper(I) iodide (141 mg, Kanto Chemicals) in methanol (5.5 ml) and pyridine (5.5 ml) was added with sodium methoxide (28% methanol solution, 1.7 ml, Wako Pure Chemical Industries) and stirred with heating at 65° C. for 24 hours. The reaction mixture was cooled to room tempe...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Ether
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1.C1CC[NH]CC1
Br-
[Cu]I.CO.N1=CC=CC=C1
65
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.C[O-]>[Cu]I.CO.N1=CC=CC=C1>COc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b56a0268b051416cac8d42612a0103b2
COc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>COc1cncc2cccc(NC3CCNCC3)c12
COC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.COC1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([O:2][CH3:1])[c:19]32)[CH2:18][CH2:17]1>>[CH3:1][O:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)[c:19]12
COc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
COc1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 96 (358 mg) and 10% hydrogen chloride/methanol solution (10 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
COc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>COc1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b5b475bd78ac49cc914631e3415b87cc
COc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12>>COc1cncc2cccc(NC3CCC(N)CC3)c12
C(C)(C)(C)OC(=O)NC1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)OC.Cl.CO>>Cl.COC1=CN=CC2=CC=CC(=C12)NC1CCC(CC1)N
CC(C)(C)OC(=O)[NH:17][CH:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([O:2][CH3:1])[c:20]32)[CH2:19][CH2:18]1>>[CH3:1][O:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][CH:16]([NH2:17])[CH2:18][CH2:19]3)[c:20]12
COc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12
COc1cncc2cccc(NC3CCC(N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 97 (372 mg) and 10% hydrogen chloride/methanol solution (10 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
COc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12>>COc1cncc2cccc(NC3CCC(N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6de56dfb6df84ba996ea22062f1fd467
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](O)CC1.COc1ccc(C(=O)O)cc1>>COc1ccc(C(=O)O[C@@H]2CC[C@H](NC(=O)OC(C)(C)C)CC2)cc1
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)O.N(=NC(=O)N(C)C)C(=O)N(C)C.C(C1=CC=C(C=C1)OC)(=O)O.C(CCC)P(CCCC)CCCC>>C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)OC(C1=CC=C(C=C1)OC)=O
[OH:9][C@H:10]1[CH2:11][CH2:12][C@H:13]([NH:14][C:15](=[O:16])[O:17][C:18]([CH3:19])([CH3:20])[CH3:21])[CH2:22][CH2:23]1.O[C:7]([c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:25][cH:24]1)=[O:8]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([C:7](=[O:8])[O:9][C@H:10]2[CH2:11][CH2:12][C@@H:13]([NH:14][C:15](=[O:16])[O:17][C:18]([CH3:19...
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](O)CC1.COc1ccc(C(=O)O)cc1
COc1ccc(C(=O)O[C@@H]2CC[C@H](NC(=O)OC(C)(C)C)CC2)cc1
null
null
C(C)(=O)OCC.O1CCCC1
Acylation
Esterification of Carboxylic Acids
e916c5b009194e30c618975b40d7a233bfcf81339e65494c4e365f67cc5e011d
12ba7405a548c6b1674f05065819c74f53f1b6165cd54e84e1f2f208042fe660
O=C(OC1CCCCC1)c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C:6]-[C:7](-[OH;D1;+0:8])-[C:9]>>[C:6]-[C:7](-[O;H0;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5])-[C:9]
96.3
[{"value": 96.3, "product": "C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)OC(C1=CC=C(C=C1)OC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
2.5
HOUR
A solution of Intermediate 35 (21.06 g), 1,1′-azobis(N,N-dimethylformamide) (64.11 g) and p-anisic acid (23.03 g, Tokyo Kasei Kogyo) in tetrahydrofuran (400 ml) was added with tri(n-butyl)phosphine (35.6 ml) at room temperature and stirred at 50° C. for 2.5 hours. The reaction mixture was cooled to room temperature, th...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary alcohol
Ester
null
null
c1ccccc1.C1CCCCC1
HO-
C(C)(=O)OCC.O1CCCC1
50
2.5
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](O)CC1.COc1ccc(C(=O)O)cc1>C(C)(=O)OCC.O1CCCC1>COc1ccc(C(=O)O[C@@H]2CC[C@H](NC(=O)OC(C)(C)C)CC2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a30f9f819ce941d6834a0c8a1332c319
COc1ccc(C(=O)O[C@@H]2CC[C@H](NC(=O)OC(C)(C)C)CC2)cc1>>CC(C)(C)OC(=O)N[C@@H]1CC[C@H](O)CC1
C(C)(=O)OCC.C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)OC(C1=CC=C(C=C1)OC)=O.[OH-].[Na+]>>C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)O
COc1ccc(C(=O)[O:13][C@H:12]2[CH2:11][CH2:10][C@@H:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:15][CH2:14]2)cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@@H:12]([OH:13])[CH2:14][CH2:15]1
COc1ccc(C(=O)O[C@@H]2CC[C@H](NC(=O)OC(C)(C)C)CC2)cc1
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](O)CC1
null
null
CO
Reduction
Hydrolysis or Hydrogenolysis of Carboxylic Esters or Thioesters
fa0d72ae7f712862012fce073f61b5242bad6a97539a947aedd819738fc0400b
2884a5654446a5b733e7d59f144021b82bebc5565dd0ff9b32ffa054af42d6b4
C1CCCCC1
C-O-c1:c:c:c(-C(=O)-[O;H0;D2;+0:1]-[C:2](-[C:3])-[C:4]):c:c:1>>[C:3]-[C:2](-[OH;D1;+0:1])-[C:4]
39.1
[{"value": 39.1, "product": "C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
1.5
HOUR
A solution of Intermediate 118 (32.92 g) in methanol (400 ml) was added with 3 N aqueous sodium hydroxide (163 ml) at room temperature and stirred at 50° C. for 1.5 hours. The reaction mixture was cooled to room temperature, then added with ethyl acetate (400 ml) and washed 4 times with 0.5 N aqueous sodium hydroxide (...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether
Secondary alcohol
c1ccccc1
null
C1CCCCC1
HO-
CO
50
1.5
COc1ccc(C(=O)O[C@@H]2CC[C@H](NC(=O)OC(C)(C)C)CC2)cc1>CO>CC(C)(C)OC(=O)N[C@@H]1CC[C@H](O)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4e85aeddbc554fecbb78e2baa0b93744
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1>>N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)Br.Cl.CO>>Cl.BrC1=CN=CC2=CC=CC(=C12)O[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:2][C@H:3]1[CH2:4][CH2:5][C@H:6]([O:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][c:16]([Br:17])[c:18]23)[CH2:19][CH2:20]1>>[NH2:2][C@H:3]1[CH2:4][CH2:5][C@H:6]([O:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][c:16]([Br:17])[c:18]23)[CH2:19][CH2:20]1
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1
N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(OC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 121 (49.4 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml). The...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1>>N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-77836b6fe0cb4c828f1476a14df81196
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1>>CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(C#N)c23)CC1
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)Br.CN(C)C=O>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)C#N
Br[c:22]1[cH:21][n:20][cH:19][c:18]2[cH:17][cH:16][cH:15][c:14]([O:13][C@H:12]3[CH2:11][CH2:10][C@H:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:27][CH2:26]3)[c:25]21>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@H:12]([O:13][c:14]2[cH:15][cH:16][cH:17][c:18]3[cH:19...
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(C#N)c23)CC1
null
[C-]#N.[Zn+2].[C-]#N.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([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2]
null
Miscellaneous
OtherReaction
c64c69b6f1d81056cbac2852296bec920cfa3f25e1fe508f94c07c888647f1dc
73a96fe5e833259ca394a42f82d6cc2ee7231bcde92d95030d2893b90c3fef76
c1cc(OC2CCCCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]>>[N;D1;H0:8]#[C:9]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
null
[]
120
CELSIUS
19
HOUR
A suspension of Intermediate 121 (113.7 mg), zinc cyanide (19.4 mg, Wako Pure Chemical Industries), tris(dibenzylideneacetone)dipalladium(0) (24.0 mg) and 1,1′-bis(diphenylphosphino)ferrocene (35.3 mg, Tokyo Kasei Kogyo) in DMF (2 ml) was stirred at 120° C. for 19 hours. The reaction mixture was concentrated under redu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Nitrile
c1ccc2cnccc2c1
c1ccc2cnccc2c1
C1CCCCC1.c1ccc2cnccc2c1
Br-
[C-]#N.[Zn+2].[C-]#N.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([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2]
120
19
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1>[C-]#N.[Zn+2].[C-]#N.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([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2]>CC(C)(C)OC(=O)N[C@@H]1CC[C@...
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ffa332e5c6fe43b5844f63ea4e7f138d
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(C#N)c23)CC1>>N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)C#N.Cl.CO>>Cl.C(#N)C1=CN=CC2=CC=CC(=C12)O[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:18][C@H:17]1[CH2:16][CH2:15][C@H:14]([O:13][c:12]2[cH:11][cH:10][cH:9][c:8]3[cH:7][n:6][cH:5][c:4]([C:3]#[N:2])[c:21]32)[CH2:20][CH2:19]1>>[N:2]#[C:3][c:4]1[cH:5][n:6][cH:7][c:8]2[cH:9][cH:10][cH:11][c:12]([O:13][C@H:14]3[CH2:15][CH2:16][C@H:17]([NH2:18])[CH2:19][CH2:20]3)[c:21]12
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(C#N)c23)CC1
N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(OC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 122 (34.9 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml). The...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(C#N)c23)CC1>>N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e6ea173fbdad4a93b30eaab9957c3e20
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cnccc23)CC1>>N[C@@H]1CC[C@@H](Oc2cccc3cnccc23)CC1
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)O[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:2][C@H:3]1[CH2:4][CH2:5][C@H:6]([O:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][cH:16][c:17]23)[CH2:18][CH2:19]1>>[NH2:2][C@H:3]1[CH2:4][CH2:5][C@H:6]([O:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][cH:16][c:17]23)[CH2:18][CH2:19]1
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cnccc23)CC1
N[C@@H]1CC[C@@H](Oc2cccc3cnccc23)CC1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(OC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 123 (59.6 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml). The...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cnccc23)CC1>>N[C@@H]1CC[C@@H](Oc2cccc3cnccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5bdc0731d83a4375b57f763a35e61dd4
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1.CCCC[C]([Sn])=C(CCCC)CCCC>>C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)Br.C(CCC)C(=C(CCCC)CCCC)[Sn].C(C)(C)(C)C1=CC(=CC(=C1O)C(C)(C)C)C>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)C=C
Br[c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([O:12][C@H:13]3[CH2:14][CH2:15][C@H:16]([NH:17][C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[CH2:25][CH2:26]3)[c:27]12.CCCC[C]([Sn])=[C:2](CCCC)[CH2:1]CCC>>[CH2:1]=[CH:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([O:12][C@H:13]3[CH2:14][CH2...
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1.CCCC[C]([Sn])=C(CCCC)CCCC
C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
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
C1(=CC=CC=C1)C
C-C Coupling
OtherReaction
82a3d2d8c84be82d43c962f9be2401515527412b6ecf104ee4b478759be8081e
27ac22ec7469bd7f39cc3c50746346e388051103704091d8380f391d425a4ebf
c1cc(OC2CCCCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7].C-C-C-C-[C;H0;D3;+0:8](-[CH2;D2;+0:9]-C-C-C)=[C](-[Sn])-C-C-C-C>>[CH2;D1;+0:9]=[CH;D2;+0:8]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
null
[]
null
null
null
null
A solution of Intermediate 121 (500 mg), tri(n-butyl)vinyltin (518 μl, Tokyo Kasei Kogyo), tetrakis(triphenylphosphine)palladium(0) (28.1 mg) and 2,6-di-tert-butyl-p-cresol (3.2 mg, Tokyo Kasei Kogyo) in toluene (10 ml) was stirred at 110° C. for 3 hours. The solvent was evaporated under reduced pressure, and the resid...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Vinyl
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1.C1CCCCC1
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.C1(=CC=CC=C1)C
null
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1.CCCC[C]([Sn])=C(CCCC)CCCC>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.C1(=CC=CC=C1)C>C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c...
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-98d12fb782ec41e3aba8ea2af660275d
C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)C=C.Cl.CO>>Cl.C(=C)C1=CN=CC2=CC=CC(=C12)O[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:17][C@H:16]1[CH2:15][CH2:14][C@H:13]([O:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([CH:2]=[CH2:1])[c:20]32)[CH2:19][CH2:18]1>>[CH2:1]=[CH:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([O:12][C@H:13]3[CH2:14][CH2:15][C@H:16]([NH2:17])[CH2:18][CH2:19]3)[c:20]12
C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(OC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 124 (83.9 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml). The...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3b14aa01c68746f3962bb1931c60dfc0
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1.N>>CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(N)c23)CC1
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)Br.C(C)(C)(C)P(C1=C(C=CC=C1)C1=CC=CC=C1)C(C)(C)C.CC(C)([O-])C.[Na+].N.O1CCOCC1>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)N
Br[c:22]1[cH:21][n:20][cH:19][c:18]2[cH:17][cH:16][cH:15][c:14]([O:13][C@H:12]3[CH2:11][CH2:10][C@H:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:26][CH2:25]3)[c:24]21.[NH3:23]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@H:12]([O:13][c:14]2[cH:15][cH:16][cH:17][c:1...
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1.N
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(N)c23)CC1
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]
null
Heteroatom Alkylation and Arylation
OtherReaction
261fd9f972974897261ca5eac8b1086caae005655bedee979c411e5b22857ba2
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1cc(OC2CCCCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7].[NH3;D0;+0:8]>>[NH2;D1;+0:8]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
null
[]
70
CELSIUS
22
HOUR
A suspension of Intermediate 121 (100 mg), tris(dibenzylideneacetone)dipalladium(0) (22.1 mg), 2-(di-tert-butylphosphino)biphenyl (33.9 mg) and sodium tert-butoxide (35.3 mg) in 0.5 N ammonia/dioxane solution (2 ml) was stirred at 70° C. for 22 hours. The reaction mixture was filtered through a Celite layer, and the so...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
C1CCCCC1.c1ccc2cnccc2c1
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]
70
22
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(Br)c23)CC1.N>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]>CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(N)c23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0a8d964313a1439fa4e37fff40891b87
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(N)c23)CC1>>Nc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)N.Cl.CO>>Cl.NC1=CN=CC2=CC=CC(=C12)O[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:17][C@H:16]1[CH2:15][CH2:14][C@H:13]([O:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([NH2:2])[c:20]32)[CH2:19][CH2:18]1>>[NH2:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([O:12][C@H:13]3[CH2:14][CH2:15][C@H:16]([NH2:17])[CH2:18][CH2:19]3)[c:20]12
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(N)c23)CC1
Nc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(OC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 8 hours) by using Intermediate 125 (36.1 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml). The...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Oc2cccc3cncc(N)c23)CC1>>Nc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-41aab4904af540338d435ca329ed8c84
C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>CCc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)C=C>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)CC
[CH2:1]=[CH:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([O:12][C@H:13]3[CH2:14][CH2:15][C@H:16]([NH:17][C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[CH2:25][CH2:26]3)[c:27]12>>[CH3:1][CH2:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([O:12][C@H:13]3[CH2:14][CH2:15][C@H:16]([NH:17][C:1...
C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
CCc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
null
[Pt]=O
CO
Reduction
Hydrogenation (double to single)
8276b4fb5ddc7d15dec6d92474e91e2dbb2fb8b81e5b5720762e5d89cb27aa69
1ccae9f2e86499601fc3421041ff4588c8e6fd53048e86c3b6ed12ae873609c0
c1cc(OC2CCCCC2)c2ccncc2c1
[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]
45.2
[{"value": 45.2, "product": "C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
HOUR
A solution of Intermediate 124 (90.5 mg) in methanol (5 ml) was added with platinum oxide (13 mg, Wako Pure Chemical Industries) and stirred for 15 hours under hydrogen atmosphere. The reaction mixture was filtered through a Celite layer, and the solvent was evaporated under reduced pressure. Then, the residue was puri...
10.6084/m9.figshare.5104873.v1
null
Vinyl
null
null
null
c1ccc2cnccc2c1.C1CCCCC1
null
[Pt]=O.CO
null
15
C=Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>[Pt]=O.CO>CCc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fe97f6283c664643b9936311d55bf07e
CCc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>CCc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)CC.Cl.CO>>Cl.C(C)C1=CN=CC2=CC=CC(=C12)O[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:17][C@H:16]1[CH2:15][CH2:14][C@H:13]([O:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([CH2:2][CH3:1])[c:20]32)[CH2:19][CH2:18]1>>[CH3:1][CH2:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([O:12][C@H:13]3[CH2:14][CH2:15][C@H:16]([NH2:17])[CH2:18][CH2:19]3)[c:20]12
CCc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
CCc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(OC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 126 (41.1 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml). The...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
CCc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>CCc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-390a66a2058b4bf8bb6c50b5617ecc7b
Cc1cncc2cccc(N)c12>>Cc1cncc2cccc(O)c12
N.O.CC1=CN=CC2=CC=CC(=C12)N.N(=O)[O-].[Na+]>>CC1=CN=CC2=CC=CC(=C12)O
N[c:10]1[cH:9][cH:8][cH:7][c:6]2[cH:5][n:4][cH:3][c:2]([CH3:1])[c:12]21>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([OH:11])[c:12]12
Cc1cncc2cccc(N)c12
Cc1cncc2cccc(O)c12
null
null
S(O)(O)(=O)=O
Functional Group Interconversion
OtherReaction
a9e88b40d19f980e8c4fbfcb1a8796d8357e51f33faec4808ce28ecbc2beaf88
ed7617b9cd113fcbf3232da782e35483fef55189a64648ab4bdbc41767cd9a80
c1ccc2cnccc2c1
N-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1>>[O;D1;H1:10]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
63.9
[{"value": 63.9, "product": "CC1=CN=CC2=CC=CC(=C12)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 4-methyl-5-aminoisoquinoline (869 mg) in concentrated sulfuric acid (8 ml) was added with sodium nitrite (379 mg) with ice cooling and stirring and stirred for 0.5 hours. The reaction mixture was added with water (12 ml) and then stirred at 130° C. for 16 hours. The reaction mixture was neutralized with 2...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Aromatic alcohol
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
null
S(O)(O)(=O)=O
null
null
Cc1cncc2cccc(N)c12>S(O)(O)(=O)=O>Cc1cncc2cccc(O)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e0052dc7514340f6aa87ab5a0aa5366d
Cc1cncc2cccc(OC3CCN(C(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(OC3CCNCC3)c12
CC1=CN=CC2=CC=CC(=C12)OC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.CC1=CN=CC2=CC=CC(=C12)OC1CCNCC1
CC(C)(C)OC(=O)[N:15]1[CH2:14][CH2:13][CH:12]([O:11][c:10]2[cH:9][cH:8][cH:7][c:6]3[cH:5][n:4][cH:3][c:2]([CH3:1])[c:18]32)[CH2:17][CH2:16]1>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([O:11][CH:12]3[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]3)[c:18]12
Cc1cncc2cccc(OC3CCN(C(=O)OC(C)(C)C)CC3)c12
Cc1cncc2cccc(OC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(OC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 128 (604 mg) and 10% hydrogen chloride/methanol solution (20 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (5 ml) and diethyl ether (15 ml). The de...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
Cc1cncc2cccc(OC3CCN(C(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(OC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f7de456d2ad64a3cbc0a43f8d6ff3aa7
Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OC1=C2C(=CN=CC2=CC=C1)C.Cl.CO>>Cl.CC1=CN=CC2=CC=CC(=C12)O[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:16][C@H:15]1[CH2:14][CH2:13][C@H:12]([O:11][c:10]2[cH:9][cH:8][cH:7][c:6]3[cH:5][n:4][cH:3][c:2]([CH3:1])[c:19]32)[CH2:18][CH2:17]1>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([O:11][C@H:12]3[CH2:13][CH2:14][C@H:15]([NH2:16])[CH2:17][CH2:18]3)[c:19]12
Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(OC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 129 (194 mg) and 10% hydrogen chloride/methanol solution (3.5 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (1 ml) and diethyl ether (3 ml). The de...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
Cc1cncc2cccc(O[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3dfa3be4800f47328a373a2f1c6c78bb
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(Cl)nccc23)CC1.N>>CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(N)nccc23)CC1
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)OC1=C2C=CN=C(C2=CC=C1)Cl.N>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)OC1=C2C=CN=C(C2=CC=C1)N
Cl[c:19]1[c:18]2[cH:17][cH:16][cH:15][c:14]([O:13][C@@H:12]3[CH2:11][CH2:10][C@H:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:26][CH2:25]3)[c:24]2[cH:23][cH:22][n:21]1.[NH3:20]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@@H:12]([O:13][c:14]2[cH:15][cH:16][cH:17][c...
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(Cl)nccc23)CC1.N
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(N)nccc23)CC1
null
null
O1CCOCC1
Heteroatom Alkylation and Arylation
OtherReaction
261fd9f972974897261ca5eac8b1086caae005655bedee979c411e5b22857ba2
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1cc(OC2CCCCC2)c2ccncc2c1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](:[c:5]):[c:6].[NH3;D0;+0:7]>>[NH2;D1;+0:7]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](:[c:5]):[c:6]
null
[]
150
CELSIUS
20
HOUR
A solution of Intermediate 130 (500 mg) in dioxane (2.5 ml) was added with 28% aqueous ammonia solution (2.5 ml) and stirred at 150° C. for 20 hours in a sealed tube. The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with dioxane (6 ml...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
C1CCCCC1.c1ccc2cnccc2c1
HCl
O1CCOCC1
150
20
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(Cl)nccc23)CC1.N>O1CCOCC1>CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(N)nccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4a4d632386d0470bab934e0fc7ebc05f
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(N)nccc23)CC1>>Nc1nccc2c(O[C@@H]3CC[C@H](N)CC3)cccc12
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)OC1=C2C=CN=C(C2=CC=C1)N.Cl.CO>>Cl.NC1=NC=CC2=C(C=CC=C12)O[C@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:14][C@H:13]1[CH2:12][CH2:11][C@@H:10]([O:9][c:8]2[c:7]3[cH:6][cH:5][n:4][c:3]([NH2:2])[c:20]3[cH:19][cH:18][cH:17]2)[CH2:16][CH2:15]1>>[NH2:2][c:3]1[n:4][cH:5][cH:6][c:7]2[c:8]([O:9][C@H:10]3[CH2:11][CH2:12][C@@H:13]([NH2:14])[CH2:15][CH2:16]3)[cH:17][cH:18][cH:19][c:20]12
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(N)nccc23)CC1
Nc1nccc2c(O[C@@H]3CC[C@H](N)CC3)cccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(OC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 131 (76 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (1 ml) and diethyl ether (3 ml). The depos...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2cccc3c(N)nccc23)CC1>>Nc1nccc2c(O[C@@H]3CC[C@H](N)CC3)cccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d189c45fbcf042a78bf55612f254a951
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1.COc1ccc(CN)cc1>>COc1ccc(CNc2nccc3c(NC4CCN(C(=O)OC(C)(C)C)CC4)cccc23)cc1
ClC1=NC=CC2=C(C=CC=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.COC1=CC=C(CN)C=C1.C(C)(C)(C)P(C1=C(C=CC=C1)C1=CC=CC=C1)C(C)(C)C.CC(C)([O-])C.[Na+]>>COC1=CC=C(CNC2=NC=CC3=C(C=CC=C23)NC2CCN(CC2)C(=O)OC(C)(C)C)C=C1
Cl[c:9]1[n:10][cH:11][cH:12][c:13]2[c:14]([NH:15][CH:16]3[CH2:17][CH2:18][N:19]([C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[CH2:27][CH2:28]3)[cH:29][cH:30][cH:31][c:32]12.[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][NH2:8])[cH:33][cH:34]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][NH:8][c:9]2[n:10][cH:11]...
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1.COc1ccc(CN)cc1
COc1ccc(CNc2nccc3c(NC4CCN(C(=O)OC(C)(C)C)CC4)cccc23)cc1
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)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
17c3dbb58f19c559a89452c2c52a32d81319b5dd6d11e225611cc478eba61c1b
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(CNc2nccc3c(NC4CCNCC4)cccc23)cc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](:[c:5]):[c:6].[NH2;D1;+0:7]-[C:8]-[c:9]>>[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[NH;D2;+0:7]-[C:8]-[c:9]):[c:4](:[c:5]):[c:6]
null
[]
70
CELSIUS
1
HOUR
A suspension of Intermediate 84 (235 mg), 4-methoxybenzylamine (110 μl), tris(dibenzylideneacetone)dipalladium(0) (30.4 mg), 2-(di-tert-butylphosphino)biphenyl (41.0 mg) and sodium tert-butoxide (93.6 mg) in toluene (4.5 ml) was stirred at 70° C. for 1 hour. The reaction mixture was filtered through a Celite layer, and...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccccc1.C1CC[NH]CC1.c1ccc2cnccc2c1
HCl
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)C
70
1
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1.COc1ccc(CN)cc1>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)C>COc1ccc(CNc2nccc3c(NC4CCN(C(=O)OC(C)(C)C)CC4)cccc23)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b3e1fac3b5b54f7b92bfe077e81f3e7b
COc1ccc(CNc2nccc3c(NC4CCN(C(=O)OC(C)(C)C)CC4)cccc23)cc1>>CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(N)nccc23)CC1
COC1=CC=C(CNC2=NC=CC3=C(C=CC=C23)NC2CCN(CC2)C(=O)OC(C)(C)C)C=C1>>NC1=NC=CC2=C(C=CC=C12)NC1CCN(CC1)C(=O)OC(C)(C)C
COc1ccc(C[NH:19][c:18]2[c:17]3[cH:16][cH:15][cH:14][c:13]([NH:12][CH:11]4[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:25][CH2:24]4)[c:23]3[cH:22][cH:21][n:20]2)cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([NH:12][c:13]2[cH:14][cH:15][cH:16][c:17]3[c:18]...
COc1ccc(CNc2nccc3c(NC4CCN(C(=O)OC(C)(C)C)CC4)cccc23)cc1
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(N)nccc23)CC1
null
null
FC(C(=O)O)(F)F
Reduction
OtherReaction
bd6cc2ddd30b209c36eb43f9e2d163a4da40f8a48bda8b578aa13caf5d4fe5dd
79272555d5bd71219cf9e8b42c4ac12a30bbf383c58cfbccf49a5a990e3653c1
c1cc(NC2CCNCC2)c2ccncc2c1
C-O-c1:c:c:c(-C-[NH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5]):c:c:1>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5]
99.6
[{"value": 99.6, "product": "NC1=NC=CC2=C(C=CC=C12)NC1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A solution of Intermediate 132 (270 mg) in 95% trifluoroacetic acid (5 ml) was stirred at 50° C. for 16 hours, and the solvent was evaporated under reduced pressure. The residue was added with dioxane (3 ml), 2 N aqueous sodium hydroxide (1 ml) and 2 di-t-butyl dicarbonate (393 mg) and stirred at room temperature for 1...
10.6084/m9.figshare.5104873.v1
null
Ether.Secondary amine
Primary amine
c1ccccc1
null
C1CC[NH]CC1.c1ccc2cnccc2c1
HO-
FC(C(=O)O)(F)F
null
1
COc1ccc(CNc2nccc3c(NC4CCN(C(=O)OC(C)(C)C)CC4)cccc23)cc1>FC(C(=O)O)(F)F>CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(N)nccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6a29741c4a614edab796fa123e380462
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(N)nccc23)CC1>>Nc1nccc2c(NC3CCNCC3)cccc12
NC1=NC=CC2=C(C=CC=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>NC1=NC=CC2=C(C=CC=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:12]1[CH2:11][CH2:10][CH:9]([NH:8][c:7]2[c:6]3[cH:5][cH:4][n:3][c:2]([NH2:1])[c:18]3[cH:17][cH:16][cH:15]2)[CH2:14][CH2:13]1>>[NH2:1][c:2]1[n:3][cH:4][cH:5][c:6]2[c:7]([NH:8][CH:9]3[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]3)[cH:15][cH:16][cH:17][c:18]12
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(N)nccc23)CC1
Nc1nccc2c(NC3CCNCC3)cccc12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
71.7
[{"value": 71.7, "product": "NC1=NC=CC2=C(C=CC=C12)NC1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 133 (199 mg) and 10% hydrogen chloride/methanol solution (3 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (1 ml) and diethyl ether (3 ml). The depo...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(N)nccc23)CC1>>Nc1nccc2c(NC3CCNCC3)cccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-89e65fdcf54141689ca1a566dc61bce4
BrCCOC1CCCCO1.c1cc(NC2CCNCC2)c2ccncc2c1>>c1cc(NC2CCN(CCOC3CCCCO3)CC2)c2ccncc2c1
CC(=O)C.Cl.C1=NC=CC2=C(C=CC=C12)NC1CCNCC1.C([O-])([O-])=O.[K+].[K+].BrCCOC1OCCCC1>>O1C(CCCC1)OCCN1CCC(CC1)NC1=C2C=CN=CC2=CC=C1
Br[CH2:9][CH2:10][O:11][CH:12]1[CH2:13][CH2:14][CH2:15][CH2:16][O:17]1.[cH:1]1[cH:2][c:3]([NH:4][CH:5]2[CH2:6][CH2:7][NH:8][CH2:18][CH2:19]2)[c:20]2[cH:21][cH:22][n:23][cH:24][c:25]2[cH:26]1>>[cH:1]1[cH:2][c:3]([NH:4][CH:5]2[CH2:6][CH2:7][N:8]([CH2:9][CH2:10][O:11][CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16][O:17]3)[CH2:18...
BrCCOC1CCCCO1.c1cc(NC2CCNCC2)c2ccncc2c1
c1cc(NC2CCN(CCOC3CCCCO3)CC2)c2ccncc2c1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1cc(NC2CCN(CCOC3CCCCO3)CC2)c2ccncc2c1
Br-[CH2;D2;+0:1]-[C:2]-[#8:3].[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:6](-[C:5]-[C:4])-[C:7]-[C:8]
null
[]
null
null
48
HOUR
A suspension of the compound of Example 20 (70 mg) and potassium carbonate (142 mg, Kokusan Chemical) in N,N-dimethylformamide (1.5 ml) was added with 2-(2-bromoethoxy)tetrahydro-2H-pyran (254 μl, Aldrich) and stirred at room temperature for 48 hours. The reaction mixture was added with acetone (10 ml), and insoluble m...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.C1CCOCC1.c1ccc2cnccc2c1
HBr
CN(C=O)C
null
48
BrCCOC1CCCCO1.c1cc(NC2CCNCC2)c2ccncc2c1>CN(C=O)C>c1cc(NC2CCN(CCOC3CCCCO3)CC2)c2ccncc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d00bddfa7b8a4ef6b23783ff72234805
BrCCOC1CCCCO1.Cc1cncc2cccc(NC3CCNCC3)c12>>Cc1cncc2cccc(NC3CCN(CCO)CC3)c12
BrCCOC1OCCCC1.Cl.CC1=CN=CC2=CC=CC(=C12)NC1CCNCC1>>Cl.OCCN1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)C
Br[CH2:16][CH2:17][O:18]C1CCCCO1.[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][CH:12]3[CH2:13][CH2:14][NH:15][CH2:19][CH2:20]3)[c:21]12>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][CH:12]3[CH2:13][CH2:14][N:15]([CH2:16][CH2:17][OH:18])[CH2:19][CH2:20]3)[c:21]12
BrCCOC1CCCCO1.Cc1cncc2cccc(NC3CCNCC3)c12
Cc1cncc2cccc(NC3CCN(CCO)CC3)c12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
92200bde28dedcd3add4f003e7f20d31008c8f0aca8f36d973aa94d011837799
0690078e74c557718340a96e117e2023ca0662eb2b391d9d3661cf44ee04bb0c
c1cc(NC2CCNCC2)c2ccncc2c1
Br-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-C1-C-C-C-C-O-1.[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8]>>[C:4]-[C:5]-[N;H0;D3;+0:6](-[CH2;D2;+0:1]-[C:2]-[OH;D1;+0:3])-[C:7]-[C:8]
null
[]
null
null
null
null
According to the method of Example 144, an alkylation reaction with 2-(2-bromoethoxy)tetrahydro-2H-pyran and a deprotection reaction were performed by using the compound of Example 106 to obtain the title compound. Conditions: See reaction.notes.procedure_details. Workup: a deprotection reaction
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Secondary amine
Primary alcohol.Tertiary amine
C1CCOCC1.C1CCNCC1
C1CC[NH]CC1
c1ccc2cnccc2c1.C1CC[NH]CC1
HBr
null
null
null
BrCCOC1CCCCO1.Cc1cncc2cccc(NC3CCNCC3)c12>>Cc1cncc2cccc(NC3CCN(CCO)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ff1c7dcd2ff349b5ac91cf5866601436
BrCCOC1CCCCO1.N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1>>OCCN[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
BrCCOC1OCCCC1.Cl.C1=NC=CC2=C(C=CC=C12)N[C@@H]1CC[C@H](CC1)N>>Cl.C1=NC=CC2=C(C=CC=C12)N[C@@H]1CC[C@H](CC1)NCCO
Br[CH2:4][CH2:3][O:2]C1CCCCO1.[NH2:5][C@H:6]1[CH2:7][CH2:8][C@H:9]([NH:10][c:11]2[cH:12][cH:13][cH:14][c:15]3[cH:16][n:17][cH:18][cH:19][c:20]23)[CH2:21][CH2:22]1>>[OH:2][CH2:3][CH2:4][NH:5][C@H:6]1[CH2:7][CH2:8][C@H:9]([NH:10][c:11]2[cH:12][cH:13][cH:14][c:15]3[cH:16][n:17][cH:18][cH:19][c:20]23)[CH2:21][CH2:22]1
BrCCOC1CCCCO1.N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
OCCN[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
ea5e2ef01067c3bff8f2185e9a1c85d176cf6a06653e5daa7dff2663a74ade66
9a9b1b205eb0298199862d313a9ef714203a0350cfdb128705dab974552275be
c1cc(NC2CCCCC2)c2ccncc2c1
Br-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-C1-C-C-C-C-O-1.[C:4]-[C:5](-[NH2;D1;+0:6])-[C:7]>>[C:4]-[C:5](-[NH;D2;+0:6]-[CH2;D2;+0:1]-[C:2]-[OH;D1;+0:3])-[C:7]
null
[]
null
null
null
null
According to the method of Example 144, an alkylation reaction with 2-(2-bromoethoxy)tetrahydro-2H-pyran and a deprotection reaction were performed by using the compound of Example 24 to obtain the title compound. Conditions: See reaction.notes.procedure_details. Workup: a deprotection reaction
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Primary amine
Primary alcohol.Secondary amine
C1CCOCC1
null
C1CCCCC1.c1ccc2cnccc2c1
HBr
null
null
null
BrCCOC1CCCCO1.N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1>>OCCN[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c1f2ade017504966a4c64c8770e8d573
BrCCOC1CCCCO1.Cc1cncc2cccc(N[C@@H]3CC[C@@H](N)CC3)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@@H](NCCO)CC3)c12
BrCCOC1OCCCC1.Cl.CC1=CN=CC2=CC=CC(=C12)N[C@@H]1CC[C@H](CC1)N>>Cl.CC1=CN=CC2=CC=CC(=C12)N[C@@H]1CC[C@H](CC1)NCCO
Br[CH2:17][CH2:18][O:19]C1CCCCO1.[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][C@H:12]3[CH2:13][CH2:14][C@H:15]([NH2:16])[CH2:20][CH2:21]3)[c:22]12>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][C@H:12]3[CH2:13][CH2:14][C@H:15]([NH:16][CH2:17][CH2:18][OH:19])[CH2:20][CH2:21...
BrCCOC1CCCCO1.Cc1cncc2cccc(N[C@@H]3CC[C@@H](N)CC3)c12
Cc1cncc2cccc(N[C@@H]3CC[C@@H](NCCO)CC3)c12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
ea5e2ef01067c3bff8f2185e9a1c85d176cf6a06653e5daa7dff2663a74ade66
9a9b1b205eb0298199862d313a9ef714203a0350cfdb128705dab974552275be
c1cc(NC2CCCCC2)c2ccncc2c1
Br-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-C1-C-C-C-C-O-1.[C:4]-[C:5](-[NH2;D1;+0:6])-[C:7]>>[C:4]-[C:5](-[NH;D2;+0:6]-[CH2;D2;+0:1]-[C:2]-[OH;D1;+0:3])-[C:7]
null
[]
null
null
null
null
According to the method of Example 144, an alkylation reaction with 2-(2-bromoethoxy)tetrahydro-2H-pyran and a deprotection reaction were performed by using the compound of Example 121 to obtain the title compound. Conditions: See reaction.notes.procedure_details. Workup: a deprotection reaction
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Primary amine
Primary alcohol.Secondary amine
C1CCOCC1
null
c1ccc2cnccc2c1.C1CCCCC1
HBr
null
null
null
BrCCOC1CCCCO1.Cc1cncc2cccc(N[C@@H]3CC[C@@H](N)CC3)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@@H](NCCO)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f848c0cd70984334a629a40bca364c48
BrCCOC1CCCCO1.N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1>>OCCN[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
BrCCOC1OCCCC1.Cl.C1=NC=CC2=C(C=CC=C12)N[C@@H]1CC[C@@H](CC1)N>>Cl.C1=NC=CC2=C(C=CC=C12)N[C@@H]1CC[C@@H](CC1)NCCO
Br[CH2:4][CH2:3][O:2]C1CCCCO1.[NH2:5][C@H:6]1[CH2:7][CH2:8][C@@H:9]([NH:10][c:11]2[cH:12][cH:13][cH:14][c:15]3[cH:16][n:17][cH:18][cH:19][c:20]23)[CH2:21][CH2:22]1>>[OH:2][CH2:3][CH2:4][NH:5][C@H:6]1[CH2:7][CH2:8][C@@H:9]([NH:10][c:11]2[cH:12][cH:13][cH:14][c:15]3[cH:16][n:17][cH:18][cH:19][c:20]23)[CH2:21][CH2:22]1
BrCCOC1CCCCO1.N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
OCCN[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
ea5e2ef01067c3bff8f2185e9a1c85d176cf6a06653e5daa7dff2663a74ade66
9a9b1b205eb0298199862d313a9ef714203a0350cfdb128705dab974552275be
c1cc(NC2CCCCC2)c2ccncc2c1
Br-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-C1-C-C-C-C-O-1.[C:4]-[C:5](-[NH2;D1;+0:6])-[C:7]>>[C:4]-[C:5](-[NH;D2;+0:6]-[CH2;D2;+0:1]-[C:2]-[OH;D1;+0:3])-[C:7]
null
[]
null
null
null
null
According to the method of Example 144, an alkylation reaction with 2-(2-bromoethoxy)tetrahydro-2H-pyran and a deprotection reaction were performed by using the compound of Example 23 to obtain the title compound. Conditions: See reaction.notes.procedure_details. Workup: a deprotection reaction
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Primary amine
Primary alcohol.Secondary amine
C1CCOCC1
null
C1CCCCC1.c1ccc2cnccc2c1
HBr
null
null
null
BrCCOC1CCCCO1.N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1>>OCCN[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-aa44ef0c05ad4a6ba243340aa196d0e5
BrCCOC1CCCCO1.Cc1cncc2cccc(N[C@@H]3CC[C@H](N)CC3)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@H](NCCO)CC3)c12
BrCCOC1OCCCC1.Cl.CC1=CN=CC2=CC=CC(=C12)N[C@@H]1CC[C@@H](CC1)N>>Cl.CC1=CN=CC2=CC=CC(=C12)N[C@@H]1CC[C@@H](CC1)NCCO
Br[CH2:17][CH2:18][O:19]C1CCCCO1.[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][C@H:12]3[CH2:13][CH2:14][C@@H:15]([NH2:16])[CH2:20][CH2:21]3)[c:22]12>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][C@H:12]3[CH2:13][CH2:14][C@@H:15]([NH:16][CH2:17][CH2:18][OH:19])[CH2:20][CH2:...
BrCCOC1CCCCO1.Cc1cncc2cccc(N[C@@H]3CC[C@H](N)CC3)c12
Cc1cncc2cccc(N[C@@H]3CC[C@H](NCCO)CC3)c12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
ea5e2ef01067c3bff8f2185e9a1c85d176cf6a06653e5daa7dff2663a74ade66
9a9b1b205eb0298199862d313a9ef714203a0350cfdb128705dab974552275be
c1cc(NC2CCCCC2)c2ccncc2c1
Br-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-C1-C-C-C-C-O-1.[C:4]-[C:5](-[NH2;D1;+0:6])-[C:7]>>[C:4]-[C:5](-[NH;D2;+0:6]-[CH2;D2;+0:1]-[C:2]-[OH;D1;+0:3])-[C:7]
null
[]
null
null
null
null
According to the method of Example 144, an alkylation reaction with 2-(2-bromoethoxy)tetrahydro-2H-pyran and a deprotection reaction were performed by using the compound of Example 120 to obtain the title compound. Conditions: See reaction.notes.procedure_details. Workup: a deprotection reaction
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Primary amine
Primary alcohol.Secondary amine
C1CCOCC1
null
c1ccc2cnccc2c1.C1CCCCC1
HBr
null
null
null
BrCCOC1CCCCO1.Cc1cncc2cccc(N[C@@H]3CC[C@H](N)CC3)c12>>Cc1cncc2cccc(N[C@@H]3CC[C@H](NCCO)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d229cb2de4d94ee3acd656b3de7ca16d
BrCCOC1CCCCO1.N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12>>N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](NCCO)CC3)c12
BrCCOC1OCCCC1.Cl.C(#N)C1=CN=CC2=CC=CC(=C12)O[C@@H]1CC[C@H](CC1)N>>Cl.C(#N)C1=CN=CC2=CC=CC(=C12)O[C@@H]1CC[C@H](CC1)NCCO
Br[CH2:19][CH2:20][O:21]C1CCCCO1.[N:2]#[C:3][c:4]1[cH:5][n:6][cH:7][c:8]2[cH:9][cH:10][cH:11][c:12]([O:13][C@H:14]3[CH2:15][CH2:16][C@H:17]([NH2:18])[CH2:22][CH2:23]3)[c:24]12>>[N:2]#[C:3][c:4]1[cH:5][n:6][cH:7][c:8]2[cH:9][cH:10][cH:11][c:12]([O:13][C@H:14]3[CH2:15][CH2:16][C@H:17]([NH:18][CH2:19][CH2:20][OH:21])[CH2:...
BrCCOC1CCCCO1.N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12
N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](NCCO)CC3)c12
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
ea5e2ef01067c3bff8f2185e9a1c85d176cf6a06653e5daa7dff2663a74ade66
9a9b1b205eb0298199862d313a9ef714203a0350cfdb128705dab974552275be
c1cc(OC2CCCCC2)c2ccncc2c1
Br-[CH2;D2;+0:1]-[C:2]-[O;H0;D2;+0:3]-C1-C-C-C-C-O-1.[C:4]-[C:5](-[NH2;D1;+0:6])-[C:7]>>[C:4]-[C:5](-[NH;D2;+0:6]-[CH2;D2;+0:1]-[C:2]-[OH;D1;+0:3])-[C:7]
null
[]
null
null
null
null
According to the method of Example 144, an alkylation reaction with 2-(2-bromoethoxy)tetrahydro-2H-pyran and a deprotection reaction were performed by using the compound of Example 134 to obtain the title compound. Conditions: See reaction.notes.procedure_details. Workup: a deprotection reaction
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Ether.Primary amine
Primary alcohol.Secondary amine
C1CCOCC1
null
c1ccc2cnccc2c1.C1CCCCC1
HBr
null
null
null
BrCCOC1CCCCO1.N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](N)CC3)c12>>N#Cc1cncc2cccc(O[C@@H]3CC[C@@H](NCCO)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-68a2a3cab0e14ea68b8e17f3298801c9
O=[N+]([O-])c1cccc2c(O)ncc(Br)c12>>Nc1cccc2c(O)ncc(Br)c12
O.O.[Sn](Cl)Cl.OC1=NC=C(C2=C(C=CC=C12)[N+](=O)[O-])Br>>OC1=NC=C(C2=C(C=CC=C12)N)Br
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][cH:5][c:6]2[c:7]([OH:8])[n:9][cH:10][c:11]([Br:12])[c:13]12>>[NH2:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[c:7]([OH:8])[n:9][cH:10][c:11]([Br:12])[c:13]12
O=[N+]([O-])c1cccc2c(O)ncc(Br)c12
Nc1cccc2c(O)ncc(Br)c12
null
null
null
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2cnccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
According to the method of Example 114, Step A, a reduction reaction with tin(II) chloride dihydrate was performed by using Intermediate 137 to obtain the title compound. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2cnccc2c1
Other
null
null
null
O=[N+]([O-])c1cccc2c(O)ncc(Br)c12>>Nc1cccc2c(O)ncc(Br)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6c378cc1f8624b089d5efbafe5b55132
Nc1cccc2c(O)ncc(Br)c12.[CH3][Sn]([CH3])([CH3])[CH3]>>Cc1cnc(O)c2cccc(N)c12
C[Sn](C)(C)C.OC1=NC=C(C2=C(C=CC=C12)N)Br>>OC1=NC=C(C2=C(C=CC=C12)N)C
Br[c:2]1[cH:3][n:4][c:5]([OH:6])[c:7]2[cH:8][cH:9][cH:10][c:11]([NH2:12])[c:13]12.[CH3][Sn]([CH3])([CH3])[CH3:1]>>[CH3:1][c:2]1[cH:3][n:4][c:5]([OH:6])[c:7]2[cH:8][cH:9][cH:10][c:11]([NH2:12])[c:13]12
Nc1cccc2c(O)ncc(Br)c12.[CH3][Sn]([CH3])([CH3])[CH3]
Cc1cnc(O)c2cccc(N)c12
null
null
null
C-C Coupling
Stille reaction_other
9226641c9ff2be6bc2e9fd20e6ce2e5c77a36942dcf6365e045325bcb58f0f54
db27eeefac0475c6d74fa10b3167e95a61caaae74e8bbafd45892452c0c3d4d6
c1ccc2cnccc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7].[CH3;D1;+0:8]-[Sn](-[CH3])(-[CH3])-[CH3]>>[CH3;D1;+0:8]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
null
[]
null
null
null
null
According to the method of Example 106, Step A, a methylation reaction with tetramethyltin was performed by using Intermediate 138 to obtain the title compound. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tin
null
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HBr.Sn
null
null
null
Nc1cccc2c(O)ncc(Br)c12.[CH3][Sn]([CH3])([CH3])[CH3]>>Cc1cnc(O)c2cccc(N)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5c825aac16db4c78bc62bbf1ee6b3093
Cc1cnc(O)c2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>Cc1cnc(O)c2cccc(N[C@@H]3CC[C@@H](N)CC3)c12
Cl.OC1=NC=C(C2=C(C=CC=C12)N[C@@H]1CC[C@H](CC1)NC(=O)OC(C)(C)C)C>>Cl.OC1=NC=C(C2=C(C=CC=C12)N[C@@H]1CC[C@H](CC1)N)C
CC(C)(C)OC(=O)[NH:17][C@H:16]1[CH2:15][CH2:14][C@H:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[c:5]([OH:6])[n:4][cH:3][c:2]([CH3:1])[c:20]32)[CH2:19][CH2:18]1>>[CH3:1][c:2]1[cH:3][n:4][c:5]([OH:6])[c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][C@H:13]3[CH2:14][CH2:15][C@H:16]([NH2:17])[CH2:18][CH2:19]3)[c:20]12
Cc1cnc(O)c2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12
Cc1cnc(O)c2cccc(N[C@@H]3CC[C@@H](N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Step A of this example, deprotection with concentrated hydrochloric acid was performed by using Intermediate 140 to obtain the title compound. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
Cc1cnc(O)c2cccc(N[C@@H]3CC[C@@H](NC(=O)OC(C)(C)C)CC3)c12>>Cc1cnc(O)c2cccc(N[C@@H]3CC[C@@H](N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ff7dca7ab98c4b5d90e0151012ef0475
Brc1cncc2ccccc12>>O=[N+]([O-])c1cccc2cncc(Br)c12
CCCCCC.BrC1=CN=CC2=CC=CC=C12.N.[N+](=O)([O-])[O-].[K+].BrC1=CN=CC2=CC=CC=C12>>BrC1=CN=CC2=CC=CC(=C12)[N+](=O)[O-]
[cH:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][c:12]([Br:13])[c:14]12>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][cH:7][c:8]2[cH:9][n:10][cH:11][c:12]([Br:13])[c:14]12
Brc1cncc2ccccc12
O=[N+]([O-])c1cccc2cncc(Br)c12
null
null
C(C)(=O)OCC.S(O)(O)(=O)=O
Functional Group Addition
OtherReaction
af041d80e34a3ce46b5eb910f230615587e5ab9eb4305ac845f1ae2dbd577a25
22f3183026a2d99c91ec0c53f0059a15c8421016bd62c8ab45281362b96dc686
c1ccc2cnccc2c1
[c:1]:[c:2]:[cH;D2;+0:3]:[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1>>[O;-;D1;H0:10]-[#7;+:11](=[O;D1;H0:12])-[c;H0;D3;+0:3](:[c:2]:[c:1]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
48.5
[{"value": 48.5, "product": "BrC1=CN=CC2=CC=CC(=C12)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
With vigorous stirring, concentrated sulfuric acid (36 ml) was added with 4-bromoisoquinoline (10.0 g, Tokyo Kasei Kogyo) to such an extent that the temperature should not exceed 10° C. and stirred for a while to attain complete dissolution. Potassium nitrate (4.9 g, Kanto Chemicals) was dissolved in concentrated sulfu...
10.6084/m9.figshare.5104873.v1
null
null
Nitro group
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
Other
C(C)(=O)OCC.S(O)(O)(=O)=O
null
null
Brc1cncc2ccccc12>C(C)(=O)OCC.S(O)(O)(=O)=O>O=[N+]([O-])c1cccc2cncc(Br)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-00b5bb361fab4493b7f9bbbc53902e9e
O=[N+]([O-])c1cccc2cncc(Br)c12>>Nc1cccc2cncc(Br)c12
[OH-].[Na+].BrC1=CN=CC2=CC=CC(=C12)[N+](=O)[O-].Cl>>BrC1=CN=CC2=CC=CC(=C12)N
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][n:8][cH:9][c:10]([Br:11])[c:12]12>>[NH2:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[cH:7][n:8][cH:9][c:10]([Br:11])[c:12]12
O=[N+]([O-])c1cccc2cncc(Br)c12
Nc1cccc2cncc(Br)c12
null
null
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2cnccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
55.9
[{"value": 55.9, "product": "BrC1=CN=CC2=CC=CC(=C12)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
12
HOUR
4-Bromo-5-nitroisoquinoline (1.0 g) synthesized as described above and stannous chloride dihydrate (4.5 g, Wako Pure Chemical Industries) were suspended in ethanol (30 ml), added with concentrated hydrochloric acid (2.3 ml) and stirred at 80° C. for 30 minutes and at room temperature for further 12 hours. The reaction ...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2cnccc2c1
Other
C(C)O
80
12
O=[N+]([O-])c1cccc2cncc(Br)c12>C(C)O>Nc1cccc2cncc(Br)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-09dfd65f903d4a53aba13fa33f376eb8
NCCCN.O=S(=O)(Cl)c1cccc2cnccc12>>NCCCNS(=O)(=O)c1cccc2cnccc12
Cl.C1=NC=CC=2C(=CC=CC12)S(=O)(=O)Cl.C(CCN)N>>C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCCCN
[NH2:1][CH2:2][CH2:3][CH2:4][NH2:5].Cl[S:6](=[O:7])(=[O:8])[c:9]1[cH:10][cH:11][cH:12][c:13]2[cH:14][n:15][cH:16][cH:17][c:18]12>>[NH2:1][CH2:2][CH2:3][CH2:4][NH:5][S:6](=[O:7])(=[O:8])[c:9]1[cH:10][cH:11][cH:12][c:13]2[cH:14][n:15][cH:16][cH:17][c:18]12
NCCCN.O=S(=O)(Cl)c1cccc2cnccc12
NCCCNS(=O)(=O)c1cccc2cnccc12
null
null
null
Miscellaneous
Sulfonamide synthesis (Schotten-Baumann) primary amine
a86b0632821e188c0a5dc5a5a2aac298ab3eccaee8a52ba46078c3d5975a290d
50f8fbf3d327483c3eeff8f6cbd4065e4c7600bb501fbe08958a5c79a0926428
c1ccc2cnccc2c1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
81.1
[{"value": 81.1, "product": "C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCCCN", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to the method of Reference Example 2, a reaction was performed by using isoquinoline-5-sulfonyl chloride hydrochloride (20 g) and 1,3-propylenediamine (22.2 g) to obtain the title compound (16.3 g). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2cnccc2c1
HCl
null
null
null
NCCCN.O=S(=O)(Cl)c1cccc2cnccc12>>NCCCNS(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ff4b8c61b8b94d78ab0ae7c76692603a
NCCCCN.O=S(=O)(Cl)c1cccc2cnccc12>>NCCCCNS(=O)(=O)c1cccc2cnccc12
Cl.C1=NC=CC=2C(=CC=CC12)S(=O)(=O)Cl.C(CCCN)N>>C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCCCCN
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][NH2:6].Cl[S:7](=[O:8])(=[O:9])[c:10]1[cH:11][cH:12][cH:13][c:14]2[cH:15][n:16][cH:17][cH:18][c:19]12>>[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][NH:6][S:7](=[O:8])(=[O:9])[c:10]1[cH:11][cH:12][cH:13][c:14]2[cH:15][n:16][cH:17][cH:18][c:19]12
NCCCCN.O=S(=O)(Cl)c1cccc2cnccc12
NCCCCNS(=O)(=O)c1cccc2cnccc12
null
null
null
Miscellaneous
Sulfonamide synthesis (Schotten-Baumann) primary amine
a86b0632821e188c0a5dc5a5a2aac298ab3eccaee8a52ba46078c3d5975a290d
50f8fbf3d327483c3eeff8f6cbd4065e4c7600bb501fbe08958a5c79a0926428
c1ccc2cnccc2c1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
61.9
[{"value": 61.9, "product": "C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCCCCN", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to the method of Reference Example 2, a reaction was performed by using isoquinoline-5-sulfonyl chloride hydrochloride (18.8 g) and 1,4-butylenediamine (25 g) to obtain the title compound (12.3 g). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2cnccc2c1
HCl
null
null
null
NCCCCN.O=S(=O)(Cl)c1cccc2cnccc12>>NCCCCNS(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3eab5bbdfa2e416eae1d6d8b01877451
CC(C)(C)OC(=O)NC1CCCC(NS(=O)(=O)c2cccc3cnccc23)C1>>NC1CCCC(NS(=O)(=O)c2cccc3cnccc23)C1
C(C)(C)(C)OC(=O)NC1CC(CCC1)NS(=O)(=O)C1=C2C=CN=CC2=CC=C1.Cl>>C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NC1CC(CCC1)N
CC(C)(C)OC(=O)[NH:1][CH:2]1[CH2:3][CH2:4][CH2:5][CH:6]([NH:7][S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][cH:14][c:15]3[cH:16][n:17][cH:18][cH:19][c:20]23)[CH2:21]1>>[NH2:1][CH:2]1[CH2:3][CH2:4][CH2:5][CH:6]([NH:7][S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][cH:14][c:15]3[cH:16][n:17][cH:18][cH:19][c:20]23)[CH2:21]1
CC(C)(C)OC(=O)NC1CCCC(NS(=O)(=O)c2cccc3cnccc23)C1
NC1CCCC(NS(=O)(=O)c2cccc3cnccc23)C1
null
null
CO
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(NC1CCCCC1)c1cccc2cnccc12
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
108.4
[{"value": 108.4, "product": "C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NC1CC(CCC1)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Intermediate 54 (6 g) obtained above was added to a 10% hydrogen chloride solution in methanol (50 ml) and stirred under reflux by heating for 1.5 hours. The solvent was evaporated under reduced pressure, and the residue was dissolved in a mixed solvent of dichloromethane and ethanol, added with saturated aqueous potas...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
CO
null
null
CC(C)(C)OC(=O)NC1CCCC(NS(=O)(=O)c2cccc3cnccc23)C1>CO>NC1CCCC(NS(=O)(=O)c2cccc3cnccc23)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-39fe4c2e1195477eb249df5a4f124b5a
CC(C)(CN)CNC(=O)OC(C)(C)C.O=S(=O)(Cl)c1cccc2cnccc12>>CC(C)(CNC(=O)OC(C)(C)C)CNS(=O)(=O)c1cccc2cnccc12
Cl.C1=NC=CC=2C(=CC=CC12)S(=O)(=O)Cl.C(C)(C)(C)OC(=O)NCC(CN)(C)C>>C(C)(C)(C)OC(=O)NCC(CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1)(C)C
[CH3:1][C:2]([CH3:3])([CH2:4][NH:5][C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12])[CH2:13][NH2:14].Cl[S:15](=[O:16])(=[O:17])[c:18]1[cH:19][cH:20][cH:21][c:22]2[cH:23][n:24][cH:25][cH:26][c:27]12>>[CH3:1][C:2]([CH3:3])([CH2:4][NH:5][C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12])[CH2:13][NH:14][S:15](=[O:16])(...
CC(C)(CN)CNC(=O)OC(C)(C)C.O=S(=O)(Cl)c1cccc2cnccc12
CC(C)(CNC(=O)OC(C)(C)C)CNS(=O)(=O)c1cccc2cnccc12
null
null
null
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
c1ccc2cnccc2c1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
97.8
[{"value": 97.8, "product": "C(C)(C)(C)OC(=O)NCC(CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to Reference Example 5, Step B, a reaction was performed by using isoquinoline-5-sulfonyl chloride hydrochloride (7.8 g) and Intermediate 56 (5.97 g) to obtain the title compound (11.36 g). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2cnccc2c1
HCl
null
null
null
CC(C)(CN)CNC(=O)OC(C)(C)C.O=S(=O)(Cl)c1cccc2cnccc12>>CC(C)(CNC(=O)OC(C)(C)C)CNS(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9bdeb39ac076409d9aa1b08b86692b72
CC(C)(CNC(=O)OC(C)(C)C)CNS(=O)(=O)c1cccc2cnccc12>>CC(C)(CN)CNS(=O)(=O)c1cccc2cnccc12
C(C)(C)(C)OC(=O)NCC(CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1)(C)C.Cl>>C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCC(CN)(C)C
CC(C)(C)OC(=O)[NH:5][CH2:4][C:2]([CH3:1])([CH3:3])[CH2:6][NH:7][S:8](=[O:9])(=[O:10])[c:11]1[cH:12][cH:13][cH:14][c:15]2[cH:16][n:17][cH:18][cH:19][c:20]12>>[CH3:1][C:2]([CH3:3])([CH2:4][NH2:5])[CH2:6][NH:7][S:8](=[O:9])(=[O:10])[c:11]1[cH:12][cH:13][cH:14][c:15]2[cH:16][n:17][cH:18][cH:19][c:20]12
CC(C)(CNC(=O)OC(C)(C)C)CNS(=O)(=O)c1cccc2cnccc12
CC(C)(CN)CNS(=O)(=O)c1cccc2cnccc12
null
null
CO
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2cnccc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
92.4
[{"value": 92.4, "product": "C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCC(CN)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to Reference Example 5, Step C, a reaction was performed by using Intermediate 57 (11 g) and 10% hydrogen chloride in methanol (80 ml) to obtain the title compound (7.58 g). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1
HO-
CO
null
null
CC(C)(CNC(=O)OC(C)(C)C)CNS(=O)(=O)c1cccc2cnccc12>CO>CC(C)(CN)CNS(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cc24d669fdfd47959b83d7a2b71561b6
CC(C)(C)OC(=O)NCc1ccc(CN)cc1.O=S(=O)(Cl)c1cccc2cnccc12>>CC(C)(C)OC(=O)NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1
Cl.C1=NC=CC=2C(=CC=CC12)S(=O)(=O)Cl.C(C)(C)(C)OC(=O)NCC1=CC=C(CN)C=C1>>C(C)(C)(C)OC(=O)NCC1=CC=C(C=C1)CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([CH2:14][NH2:15])[cH:29][cH:30]1.Cl[S:16](=[O:17])(=[O:18])[c:19]1[cH:20][cH:21][cH:22][c:23]2[cH:24][n:25][cH:26][cH:27][c:28]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([CH2:14][NH...
CC(C)(C)OC(=O)NCc1ccc(CN)cc1.O=S(=O)(Cl)c1cccc2cnccc12
CC(C)(C)OC(=O)NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1
null
null
null
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
O=S(=O)(NCc1ccccc1)c1cccc2cnccc12
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[NH2;D1;+0:7]-[C:8]-[c:9]>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[NH;D2;+0:7]-[C:8]-[c:9])-[c:4](:[c:5]):[c:6]
82.7
[{"value": 82.7, "product": "C(C)(C)(C)OC(=O)NCC1=CC=C(C=C1)CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to Reference Example 5, Step B, a reaction was performed by using isoquinoline-5-sulfonyl chloride hydrochloride (10 g) and Intermediate 59 (8.96 g) to obtain the title compound (13.39 g). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccccc1.c1ccc2cnccc2c1
HCl
null
null
null
CC(C)(C)OC(=O)NCc1ccc(CN)cc1.O=S(=O)(Cl)c1cccc2cnccc12>>CC(C)(C)OC(=O)NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-91463f1115d148529346c0f15f210d9b
CC(C)(C)OC(=O)NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1>>NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1
C(C)(C)(C)OC(=O)NCC1=CC=C(C=C1)CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1.Cl>>C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCC1=CC=C(C=C1)CN
CC(C)(C)OC(=O)[NH:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][NH:8][S:9](=[O:10])(=[O:11])[c:12]2[cH:13][cH:14][cH:15][c:16]3[cH:17][n:18][cH:19][cH:20][c:21]23)[cH:22][cH:23]1>>[NH2:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][NH:8][S:9](=[O:10])(=[O:11])[c:12]2[cH:13][cH:14][cH:15][c:16]3[cH:17][n:18][cH:19][cH:20][c:21]23)...
CC(C)(C)OC(=O)NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1
NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1
null
null
CO
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(NCc1ccccc1)c1cccc2cnccc12
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[c:3]>>[NH2;D1;+0:1]-[C:2]-[c:3]
80.5
[{"value": 80.5, "product": "C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCC1=CC=C(C=C1)CN", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to Reference Example 5, Step C, a reaction was performed by using Intermediate 60 (6 g) and 10% hydrogen chloride in methanol (20 ml) to obtain the title compound (3.7 g). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
CO
null
null
CC(C)(C)OC(=O)NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1>CO>NCc1ccc(CNS(=O)(=O)c2cccc3cnccc23)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5c0b777ddedc4173bf1e910f3e6f9fd8
CC(C)(C)OC(=O)NCc1cccc(CN)c1.O=S(=O)(Cl)c1cccc2cnccc12>>CC(C)(C)OC(=O)NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1
Cl.C1=NC=CC=2C(=CC=CC12)S(=O)(=O)Cl.C(C)(C)(C)OC(=O)NCC=1C=C(CN)C=CC1>>C(C)(C)(C)OC(=O)NCC1=CC(=CC=C1)CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][c:10]1[cH:11][cH:12][cH:13][c:14]([CH2:15][NH2:16])[cH:30]1.Cl[S:17](=[O:18])(=[O:19])[c:20]1[cH:21][cH:22][cH:23][c:24]2[cH:25][n:26][cH:27][cH:28][c:29]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][c:10]1[cH:11][cH:12][cH:13][c:14]([CH2...
CC(C)(C)OC(=O)NCc1cccc(CN)c1.O=S(=O)(Cl)c1cccc2cnccc12
CC(C)(C)OC(=O)NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1
null
null
null
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
O=S(=O)(NCc1ccccc1)c1cccc2cnccc12
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[NH2;D1;+0:7]-[C:8]-[c:9]>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[NH;D2;+0:7]-[C:8]-[c:9])-[c:4](:[c:5]):[c:6]
78.1
[{"value": 78.1, "product": "C(C)(C)(C)OC(=O)NCC1=CC(=CC=C1)CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to Reference Example 5, Step B, a reaction was performed by using isoquinoline-5-sulfonyl chloride hydrochloride (9 g) and Intermediate 62 (8 g) to obtain the title compound (11.3 g). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccccc1.c1ccc2cnccc2c1
HCl
null
null
null
CC(C)(C)OC(=O)NCc1cccc(CN)c1.O=S(=O)(Cl)c1cccc2cnccc12>>CC(C)(C)OC(=O)NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-45adba3b20e14f428e038d8658406cee
CC(C)(C)OC(=O)NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1>>NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1
C(C)(C)(C)OC(=O)NCC1=CC(=CC=C1)CNS(=O)(=O)C1=C2C=CN=CC2=CC=C1.Cl>>C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCC1=CC(=CC=C1)CN
CC(C)(C)OC(=O)[NH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][c:7]([CH2:8][NH:9][S:10](=[O:11])(=[O:12])[c:13]2[cH:14][cH:15][cH:16][c:17]3[cH:18][n:19][cH:20][cH:21][c:22]23)[cH:23]1>>[NH2:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][c:7]([CH2:8][NH:9][S:10](=[O:11])(=[O:12])[c:13]2[cH:14][cH:15][cH:16][c:17]3[cH:18][n:19][cH:20][cH:21][c...
CC(C)(C)OC(=O)NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1
NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1
null
null
CO
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(NCc1ccccc1)c1cccc2cnccc12
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[c:3]>>[NH2;D1;+0:1]-[C:2]-[c:3]
81
[{"value": 81.0, "product": "C1=NC=CC2=C(C=CC=C12)S(=O)(=O)NCC1=CC(=CC=C1)CN", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
According to Reference Example 5, Step C, a reaction was performed by using Intermediate 63 (5 g) and 10% hydrogen chloride in methanol (20 ml) to obtain the title compound (3.1 g). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
CO
null
null
CC(C)(C)OC(=O)NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1>CO>NCc1cccc(CNS(=O)(=O)c2cccc3cnccc23)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9a2925c670fe42288d32beb72b10d9f5
C=O.O=C1C=CC(=O)N1>>O=C1C=C(CO)C(=O)N1
C1(C=CC(N1)=O)=O.C=O.[OH-].[Na+]>>OCC=1C(=O)NC(C1)=O
[CH2:5]=[O:6].[O:1]=[C:2]1[CH:3]=[CH:4][C:7](=[O:8])[NH:9]1>>[O:1]=[C:2]1[CH:3]=[C:4]([CH2:5][OH:6])[C:7](=[O:8])[NH:9]1
C=O.O=C1C=CC(=O)N1
O=C1C=C(CO)C(=O)N1
null
null
null
C-C Coupling
OtherReaction
17a8683b74042d2cc6981b4023bdc52e578574819630a5c7a7864de64f51c3f1
4396295d899f5d4f5de2e844a80fc7d194b4da158f49df3d2717206b401b59bd
O=C1C=CC(=O)N1
[CH2;D1;+0:1]=[O;H0;D1;+0:2].[O;D1;H0:3]=[C:4]1-[#7:5]-[C:6](=[O;D1;H0:7])-[CH;D2;+0:8]=[C:9]-1>>[O;D1;H0:3]=[C:4]1-[#7:5]-[C:6](=[O;D1;H0:7])-[C;H0;D3;+0:8](-[CH2;D2;+0:1]-[OH;D1;+0:2])=[C:9]-1
null
[]
null
null
null
null
24 Parts of maleimide (manufactured by Aldrich Corporation), 21 parts of 35% HCOH (manufactured by Wako Pure Chemical Industries, Ltd.) and 0.7 parts of a 5% aqueous NaOH solution are placed in a reactor and reacted at 40° C. for 2 hours. As a result, a white crystal of hydroxymethylmaleimide precipitates. This white c...
10.6084/m9.figshare.5104873.v1
null
Formaldehyde
Primary alcohol
C1=CCNC1
C1=CCNC1
C1=CCNC1
null
null
null
null
C=O.O=C1C=CC(=O)N1>>O=C1C=C(CO)C(=O)N1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-62574a4f57594484b87becc8b7f760e8
CCCCCC(O)Br.O=S(=O)([O-])c1ccc(O)cc1>>O=S(=O)([O-])c1ccc(OCCCCCCO)cc1
[Na+].OC1=CC=C(C=C1)S(=O)(=O)[O-].[OH-].[K+].BrC(CCCCC)O>>OCCCCCCOC1=CC=C(C=C1)S(=O)(=O)[O-].[Na+]
Br[CH:10]([CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])[OH:16].[O:1]=[S:2](=[O:3])([O-:4])[c:5]1[cH:6][cH:7][c:8]([OH:9])[cH:17][cH:18]1>>[O:1]=[S:2](=[O:3])([O-:4])[c:5]1[cH:6][cH:7][c:8]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][OH:16])[cH:17][cH:18]1
CCCCCC(O)Br.O=S(=O)([O-])c1ccc(O)cc1
O=S(=O)([O-])c1ccc(OCCCCCCO)cc1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
2a9380ebb68334989924756cf01b7949046a4f7a65a764f1d76e39ed500565f9
2786f500c47f12973cdffc6c715f1d0ddaf160e62af6ac2ce87986b5e7d6597e
c1ccccc1
Br-[CH;D3;+0:1](-[OH;D1;+0:2])-[C:3]-[C:4]-[C:5]-[C:6]-[CH3;D1;+0:7].[OH;D1;+0:8]-[c:9](:[c:10]):[c:11]>>[OH;D1;+0:2]-[CH2;D2;+0:7]-[C:6]-[C:5]-[C:4]-[C:3]-[CH2;D2;+0:1]-[O;H0;D2;+0:8]-[c:9](:[c:10]):[c:11]
98.8
[{"value": 92.0, "product": "OCCCCCCOC1=CC=C(C=C1)S(=O)(=O)[O-].[Na+]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.8, "product": "OCCCCCCOC1=CC=C(C=C1)S(=O)(=O)[O-].[Na+]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Into a three-necked round-bottom flask equipped with a magnetic stirring bar and a reflux condenser were added 4-hydroxybenzenesulfonicacid sodium salt (30.0 grams (g), 0.13 mol), potassium hydroxide (9.0 g, 0.16 mol) and distilled water (60 milliliter (ml)). 1-Bromohexanol (23.16 g, 0.13 mol) dissolved in ethanol (50 ...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Secondary alcohol.Aromatic alcohol
Ether.Primary alcohol
null
null
c1ccccc1
HBr
C(C)O
null
null
CCCCCC(O)Br.O=S(=O)([O-])c1ccc(O)cc1>C(C)O>O=S(=O)([O-])c1ccc(OCCCCCCO)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-327e3218e975482ebbe892dcbab483af
CC(C)(C)c1ccc(O)c(C(C)(C)C)c1.CC(C)c1cccc(C(C)C)c1N>>CC(C)c1cccc(C(C)C)c1N=Nc1cc(C(C)(C)C)cc(C(C)(C)C)c1O
C(C)(C)C1=C(N)C(=CC=C1)C(C)C.N1=CC=CC=C1.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O.[OH-].[Na+].C1(=CC=CC=C1)[O-]>>C(C)(C)C1=C(C(=CC=C1)C(C)C)N=NC1=C(C(=CC(=C1)C(C)(C)C)C(C)(C)C)O
[cH:15]1[cH:16][c:17]([C:18]([CH3:19])([CH3:20])[CH3:21])[cH:22][c:23]([C:24]([CH3:25])([CH3:26])[CH3:27])[c:28]1[OH:29].[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][c:8]([CH:9]([CH3:10])[CH3:11])[c:12]1[NH2:13]>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][c:8]([CH:9]([CH3:10])[CH3:11])[c:12]1[N:13]=[N:14][c:15]1[...
CC(C)(C)c1ccc(O)c(C(C)(C)C)c1.CC(C)c1cccc(C(C)C)c1N
CC(C)c1cccc(C(C)C)c1N=Nc1cc(C(C)(C)C)cc(C(C)(C)C)c1O
null
null
O.C1(=CC=CC=C1)C
Functional Group Addition
OtherReaction
4dfa1e0075917e3f76a2c771d85af2eb7328e8c1dacc2fef053ab9d7871727bb
369e32a405523c63be3b198dc14b1fa8567bb17806d598f8dc85ecca177f9307
c1ccc(N=Nc2ccccc2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H1:5]-[c:6](:[c:7]):[cH;D2;+0:8]:[c:9]:[c:10]>>[O;D1;H1:5]-[c:6](:[c:7]):[c;H0;D3;+0:8](-[#7:11]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]):[c:9]:[c:10]
null
[]
null
null
null
null
This phenol was prepared, as described for above, from a theoretical yield of 7.4 mmol of diazotized 2,6-diisopropylaniline and a phenolate solution comprised of 2,4-Ditertbutylphenol (1.42 g), water (15 mL), NaOH (0.5 g), pyridine (3 mL), and toluene (6 mL) Yield=0.98 g (36%). Conditions: See reaction.notes.procedure_...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Diazene
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
Other
O.C1(=CC=CC=C1)C
null
null
CC(C)(C)c1ccc(O)c(C(C)(C)C)c1.CC(C)c1cccc(C(C)C)c1N>O.C1(=CC=CC=C1)C>CC(C)c1cccc(C(C)C)c1N=Nc1cc(C(C)(C)C)cc(C(C)(C)C)c1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-966493f923fe4472bb4fc0c0429b9e71
CC(C)c1cccc(C(C)C)c1N.Cc1ccc(O)c(-c2c3ccccc3cc3ccccc23)c1>>Cc1cc(N=Nc2c(C(C)C)cccc2C(C)C)c(O)c(-c2c3ccccc3cc3ccccc23)c1
C(C)(C)C1=C(N)C(=CC=C1)C(C)C.N1=CC=CC=C1.C1=CC=CC2=CC3=CC=CC=C3C(=C12)C1=C(C=CC(=C1)C)O.[OH-].[Na+].C1(=CC=CC=C1)[O-]>>C(C)(C)C1=C(C(=CC=C1)C(C)C)N=NC1=C(C(=CC(=C1)C)C=1C2=CC=CC=C2C=C2C=CC=CC12)O
[NH2:6][c:7]1[c:8]([CH:9]([CH3:10])[CH3:11])[cH:12][cH:13][cH:14][c:15]1[CH:16]([CH3:17])[CH3:18].[CH3:1][c:2]1[cH:3][cH:4][c:19]([OH:20])[c:21](-[c:22]2[c:23]3[cH:24][cH:25][cH:26][cH:27][c:28]3[cH:29][c:30]3[cH:31][cH:32][cH:33][cH:34][c:35]23)[cH:36]1>>[CH3:1][c:2]1[cH:3][c:4]([N:5]=[N:6][c:7]2[c:8]([CH:9]([CH3:10])...
CC(C)c1cccc(C(C)C)c1N.Cc1ccc(O)c(-c2c3ccccc3cc3ccccc23)c1
Cc1cc(N=Nc2c(C(C)C)cccc2C(C)C)c(O)c(-c2c3ccccc3cc3ccccc23)c1
null
null
O.C1=CC=CC=C1
Functional Group Addition
OtherReaction
4dfa1e0075917e3f76a2c771d85af2eb7328e8c1dacc2fef053ab9d7871727bb
369e32a405523c63be3b198dc14b1fa8567bb17806d598f8dc85ecca177f9307
c1ccc(N=Nc2cccc(-c3c4ccccc4cc4ccccc34)c2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H1:5]-[c:6](:[c:7]):[cH;D2;+0:8]:[c:9]:[c:10]>>[O;D1;H1:5]-[c:6](:[c:7]):[c;H0;D3;+0:8](-[#7:11]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]):[c:9]:[c:10]
null
[]
null
null
null
null
This phenol was prepared, as described above, from a theoretical yield of 3.9 mmol of diazotized 2,6-diisopropylaniline and a phenolate solution comprised of 2-(9-Anthracenyl)-4-methylphenol (0.63 g), water (20 mL), NaOH (20 mmol), pyridine (2 mL), and benzene (4 mL). In this case, the product was eluted with ether:hex...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Diazene
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1.c1ccc2cc3ccccc3cc2c1
Other
O.C1=CC=CC=C1
null
null
CC(C)c1cccc(C(C)C)c1N.Cc1ccc(O)c(-c2c3ccccc3cc3ccccc23)c1>O.C1=CC=CC=C1>Cc1cc(N=Nc2c(C(C)C)cccc2C(C)C)c(O)c(-c2c3ccccc3cc3ccccc23)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-45f72defb4ae417cbbd01a6cb99366f1
COc1cscc1OC.C[C@H](O)CO>>CC1COc2cscc2O1
COC1=CSC=C1OC.C([C@H](C)O)O.C(C)(=O)OCC>>CC1COC=2C(O1)=CSC2
CO[c:5]1[cH:6][s:7][cH:8][c:9]1OC.[CH3:1][C@@H:2]([CH2:3][OH:4])[OH:10]>>[CH3:1][CH:2]1[CH2:3][O:4][c:5]2[cH:6][s:7][cH:8][c:9]2[O:10]1
COc1cscc1OC.C[C@H](O)CO
CC1COc2cscc2O1
null
O.C1(=CC=C(C=C1)S(=O)(=O)O)C
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
27a88f912a54d2a9c5080f339a9b1dc6565f1d8c89ad4e25d07c18a8cc4561ec
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
c1scc2c1OCCO2
C-O-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:1-O-C.[C;D1;H3:6]-[C@H;D3;+0:7](-[OH;D1;+0:8])-[C:9]-[OH;D1;+0:10]>>[C;D1;H3:6]-[CH;D3;+0:7]1-[C:9]-[O;H0;D2;+0:10]-[c;H0;D3;+0:1]2:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:2-[O;H0;D2;+0:8]-1
69.5
[{"value": 69.5, "product": "CC1COC=2C(O1)=CSC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3,4-dimethoxythiophene (5.18 g), (S)-1,2-propanediol (3.0 g) and p-toluenesulfonic acid monohydrate (100 mg) in toluene (50 ml) was heated at 95° C. during which a continuous stream of nitrogen was passed over the solution. After 30 h the reaction mixture was poured into ethyl acetate, washed with NaHCO3 ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
c1ccsc1
c1scc2c1OCCO2
c1scc2c1OCCO2
HO-
O.C1(=CC=C(C=C1)S(=O)(=O)O)C.C1(=CC=CC=C1)C
null
null
COc1cscc1OC.C[C@H](O)CO>O.C1(=CC=C(C=C1)S(=O)(=O)O)C.C1(=CC=CC=C1)C>CC1COc2cscc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-893c7cabb2234d5d8d2cba94eaa12eb3
CC(O)CO.COc1cscc1OC>>CC1COc2cscc2O1
COC1=CSC=C1OC.C(C(C)O)O>>CC1COC=2C(O1)=CSC2
[CH3:1][CH:2]([CH2:3][OH:4])[OH:10].CO[c:5]1[cH:6][s:7][cH:8][c:9]1OC>>[CH3:1][CH:2]1[CH2:3][O:4][c:5]2[cH:6][s:7][cH:8][c:9]2[O:10]1
CC(O)CO.COc1cscc1OC
CC1COc2cscc2O1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
27a88f912a54d2a9c5080f339a9b1dc6565f1d8c89ad4e25d07c18a8cc4561ec
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
c1scc2c1OCCO2
C-O-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:1-O-C.[C;D1;H3:6]-[C:7](-[OH;D1;+0:8])-[C:9]-[OH;D1;+0:10]>>[C;D1;H3:6]-[C:7]1-[C:9]-[O;H0;D2;+0:10]-[c;H0;D3;+0:1]2:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:2-[O;H0;D2;+0:8]-1
null
[]
null
null
null
null
Racemic 2-methyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine was synthesized by transetherification of 3,4-dimethoxythiophene with racemic 1,2-propanediol as described in COMPARATIVE EXAMPLE 1. It was characterized by GC-MS and H-NMR-spectroscopy, and exhibited no optical rotation. Conditions: See reaction.notes.procedure_de...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
c1ccsc1
c1scc2c1OCCO2
c1scc2c1OCCO2
HO-
null
null
null
CC(O)CO.COc1cscc1OC>>CC1COc2cscc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-38c21bccac1c466a9310412c0c189a9d
CCCCCCCCCC[C@H](O)CO.COc1cscc1OC>>CCCCCCCCCCC1COc2cscc2O1
N#N.COC1=CSC=C1OC.C1(=CC=CC=C1)C.C([C@H](CCCCCCCCCC)O)O>>C(CCCCCCCCC)C1COC=2C(O1)=CSC2
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C@@H:11]([CH2:12][OH:13])[OH:19].CO[c:14]1[cH:15][s:16][cH:17][c:18]1OC>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH:11]1[CH2:12][O:13][c:14]2[cH:15][s:16][cH:17][c:18]2[O:19]1
CCCCCCCCCC[C@H](O)CO.COc1cscc1OC
CCCCCCCCCCC1COc2cscc2O1
null
O.C1(=CC=C(C=C1)S(=O)(=O)O)C
C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
27a88f912a54d2a9c5080f339a9b1dc6565f1d8c89ad4e25d07c18a8cc4561ec
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
c1scc2c1OCCO2
C-O-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:1-O-C.[C:6]-[C:7]-[C@H;D3;+0:8](-[OH;D1;+0:9])-[C:10]-[OH;D1;+0:11]>>[C:6]-[C:7]-[CH;D3;+0:8]1-[C:10]-[O;H0;D2;+0:11]-[c;H0;D3;+0:1]2:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:2-[O;H0;D2;+0:9]-1
68.8
[{"value": 68.8, "product": "C(CCCCCCCCC)C1COC=2C(O1)=CSC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3,4-dimethoxythiophene (1.90 g), toluene (30 ml), (S)-1,2-dodecanediol (2.50 g) and p-toluenesulfonic acid monohydrate (100 mg) was heated at 95° C., continuously leading a N2-stream over the solution. After 24 h the reaction mixture was poured into ethyl acetate, washed with NaHCO3 and the organic phase ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
c1ccsc1
c1scc2c1OCCO2
c1scc2c1OCCO2
HO-
O.C1(=CC=C(C=C1)S(=O)(=O)O)C.C(C)(=O)OCC
null
null
CCCCCCCCCC[C@H](O)CO.COc1cscc1OC>O.C1(=CC=C(C=C1)S(=O)(=O)O)C.C(C)(=O)OCC>CCCCCCCCCCC1COc2cscc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ea20d853f7c44473a5eaaef5b2e39442
CCCCCCCCCCC(O)CO.COc1cscc1OC>>CCCCCCCCCCC1COc2cscc2O1
COC1=CSC=C1OC.C(C(CCCCCCCCCC)O)O>>C(CCCCCCCCC)C1COC=2C(O1)=CSC2
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH:11]([CH2:12][OH:13])[OH:19].CO[c:14]1[cH:15][s:16][cH:17][c:18]1OC>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH:11]1[CH2:12][O:13][c:14]2[cH:15][s:16][cH:17][c:18]2[O:19]1
CCCCCCCCCCC(O)CO.COc1cscc1OC
CCCCCCCCCCC1COc2cscc2O1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
27a88f912a54d2a9c5080f339a9b1dc6565f1d8c89ad4e25d07c18a8cc4561ec
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
c1scc2c1OCCO2
C-O-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:1-O-C.[C:6]-[C:7](-[OH;D1;+0:8])-[C:9]-[OH;D1;+0:10]>>[C:6]-[C:7]1-[C:9]-[O;H0;D2;+0:10]-[c;H0;D3;+0:1]2:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:2-[O;H0;D2;+0:8]-1
null
[]
null
null
null
null
Racemic 2-n-decyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine was synthesized by transetherification of 3,4-dimethoxythiophene with racemic 1,2-dodecanediol as described in EXAMPLE 1. It was characterized by GC-MS and H-NMR-spectroscopy, and exhibited no optical rotation. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
c1ccsc1
c1scc2c1OCCO2
c1scc2c1OCCO2
HO-
null
null
null
CCCCCCCCCCC(O)CO.COc1cscc1OC>>CCCCCCCCCCC1COc2cscc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-519add250e7d4ab9915edef34623bdcd
CCCCCC[C@H](O)CO.COc1cscc1OC>>CCCCCCC1COc2cscc2O1
COC1=CSC=C1OC.C([C@H](CCCCCC)O)O>>C(CCCCC)C1COC=2C(O1)=CSC2
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C@@H:7]([CH2:8][OH:9])[OH:15].CO[c:10]1[cH:11][s:12][cH:13][c:14]1OC>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH:7]1[CH2:8][O:9][c:10]2[cH:11][s:12][cH:13][c:14]2[O:15]1
CCCCCC[C@H](O)CO.COc1cscc1OC
CCCCCCC1COc2cscc2O1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
27a88f912a54d2a9c5080f339a9b1dc6565f1d8c89ad4e25d07c18a8cc4561ec
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
c1scc2c1OCCO2
C-O-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:1-O-C.[C:6]-[C:7]-[C@H;D3;+0:8](-[OH;D1;+0:9])-[C:10]-[OH;D1;+0:11]>>[C:6]-[C:7]-[CH;D3;+0:8]1-[C:10]-[O;H0;D2;+0:11]-[c;H0;D3;+0:1]2:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:2-[O;H0;D2;+0:9]-1
null
[]
null
null
null
null
Chiral 2-n-hexyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine was synthesized by transetherification of 3,4-dimethoxythiophene with (S)-1,2-octanediol and purified to a purity of 99.69% as described in INVENTION EXAMPLE 1. It was characterized by GC-MS and 1H-NMR-spectroscopy, and exhibited a specific rotation of −100° at 25°...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
c1ccsc1
c1scc2c1OCCO2
c1scc2c1OCCO2
HO-
null
null
null
CCCCCC[C@H](O)CO.COc1cscc1OC>>CCCCCCC1COc2cscc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6b01b300406b47048991d30fbf312366
CCCCCCC(O)CO.COc1cscc1OC>>CCCCCCC1COc2cscc2O1
COC1=CSC=C1OC.C(C(CCCCCC)O)O>>C(CCCCC)C1COC=2C(O1)=CSC2
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH:7]([CH2:8][OH:9])[OH:15].CO[c:10]1[cH:11][s:12][cH:13][c:14]1OC>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH:7]1[CH2:8][O:9][c:10]2[cH:11][s:12][cH:13][c:14]2[O:15]1
CCCCCCC(O)CO.COc1cscc1OC
CCCCCCC1COc2cscc2O1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
27a88f912a54d2a9c5080f339a9b1dc6565f1d8c89ad4e25d07c18a8cc4561ec
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
c1scc2c1OCCO2
C-O-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:1-O-C.[C:6]-[C:7](-[OH;D1;+0:8])-[C:9]-[OH;D1;+0:10]>>[C:6]-[C:7]1-[C:9]-[O;H0;D2;+0:10]-[c;H0;D3;+0:1]2:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:2-[O;H0;D2;+0:8]-1
null
[]
null
null
null
null
Racemic 2-n-hexyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine was synthesized by transetherification of 3,4-dimethoxythiophene with racemic 1,2-octanediol as described in EXAMPLE 1. It was characterized by GC-MS and 1H-NMR-spectroscopy, and exhibited no optical rotation. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
c1ccsc1
c1scc2c1OCCO2
c1scc2c1OCCO2
HO-
null
null
null
CCCCCCC(O)CO.COc1cscc1OC>>CCCCCCC1COc2cscc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0c7091e2d6c4451cab60f2773711d577
CCCCCCCC[C@H](O)CO.COc1cscc1OC>>CCCCCCCCC1COc2cscc2O1
COC1=CSC=C1OC.C([C@H](CCCCCCCC)O)O>>C(CCCCCCC)C1COC=2C(O1)=CSC2
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][C@@H:9]([CH2:10][OH:11])[OH:17].CO[c:12]1[cH:13][s:14][cH:15][c:16]1OC>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH:9]1[CH2:10][O:11][c:12]2[cH:13][s:14][cH:15][c:16]2[O:17]1
CCCCCCCC[C@H](O)CO.COc1cscc1OC
CCCCCCCCC1COc2cscc2O1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
27a88f912a54d2a9c5080f339a9b1dc6565f1d8c89ad4e25d07c18a8cc4561ec
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
c1scc2c1OCCO2
C-O-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:1-O-C.[C:6]-[C:7]-[C@H;D3;+0:8](-[OH;D1;+0:9])-[C:10]-[OH;D1;+0:11]>>[C:6]-[C:7]-[CH;D3;+0:8]1-[C:10]-[O;H0;D2;+0:11]-[c;H0;D3;+0:1]2:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:2-[O;H0;D2;+0:9]-1
null
[]
null
null
null
null
Chiral 2-n-octyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine was synthesized by transetherification of 3,4-dimethoxythiophene with (S)-1,2-decanediol and purified to a purity of 99.24% as described in INVENTION EXAMPLE 1. It was characterized by GC-MS and 1H-NMR-spectroscopy, and exhibited a specific rotation of −88° at 25° ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
c1ccsc1
c1scc2c1OCCO2
c1scc2c1OCCO2
HO-
null
null
null
CCCCCCCC[C@H](O)CO.COc1cscc1OC>>CCCCCCCCC1COc2cscc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1304dd98d8844e43abc758850cf83b9e
CCCCCCCCCCCC[C@H](O)CO.COc1cscc1OC>>CCCCCCCCCCCCC1COc2cscc2O1
COC1=CSC=C1OC.C([C@H](CCCCCCCCCCCC)O)O>>C(CCCCCCCCCCC)C1COC=2C(O1)=CSC2
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C@@H:13]([CH2:14][OH:15])[OH:21].CO[c:16]1[cH:17][s:18][cH:19][c:20]1OC>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH:13]1[CH2:14][O:15][c:16]2[cH:17][s:18][cH:19][c:20]2[O:21]1
CCCCCCCCCCCC[C@H](O)CO.COc1cscc1OC
CCCCCCCCCCCCC1COc2cscc2O1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
27a88f912a54d2a9c5080f339a9b1dc6565f1d8c89ad4e25d07c18a8cc4561ec
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
c1scc2c1OCCO2
C-O-[c;H0;D3;+0:1]1:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:1-O-C.[C:6]-[C:7]-[C@H;D3;+0:8](-[OH;D1;+0:9])-[C:10]-[OH;D1;+0:11]>>[C:6]-[C:7]-[CH;D3;+0:8]1-[C:10]-[O;H0;D2;+0:11]-[c;H0;D3;+0:1]2:[c:2]:[#16;a:3]:[c:4]:[c;H0;D3;+0:5]:2-[O;H0;D2;+0:9]-1
null
[]
null
null
null
null
Chiral 2-n-dodecyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine was synthesized by transetherification of 3,4-dimethoxythiophene with (S)-1,2-tetradecanediol and purified to a purity of 98.01% as described in INVENTION EXAMPLE 1. It was characterized by GC-MS and 1H-NMR-spectroscopy, and exhibited a specific rotation of −65° ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
c1ccsc1
c1scc2c1OCCO2
c1scc2c1OCCO2
HO-
null
null
null
CCCCCCCCCCCC[C@H](O)CO.COc1cscc1OC>>CCCCCCCCCCCCC1COc2cscc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0fb2734542694c16affef6dddddfd246
CCOC(=O)C(Br)(Br)C(=O)OCC.Oc1ccccc1O>>CCOC(=O)C1(C(=O)OCC)Oc2ccccc2O1
C=1(O)C(O)=CC=CC1.BrC(C(=O)OCC)(C(=O)OCC)Br.C([O-])([O-])=O.[K+].[K+]>>C(C)OC(=O)C1(OC2=C(O1)C=CC=C2)C(=O)OCC
Br[C:6](Br)([C:4]([O:3][CH2:2][CH3:1])=[O:5])[C:7](=[O:8])[O:9][CH2:10][CH3:11].[OH:12][c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[OH:19]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]1([C:7](=[O:8])[O:9][CH2:10][CH3:11])[O:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]2[O:19]1
CCOC(=O)C(Br)(Br)C(=O)OCC.Oc1ccccc1O
CCOC(=O)C1(C(=O)OCC)Oc2ccccc2O1
null
null
CC(=O)C
Heteroatom Alkylation and Arylation
OtherReaction
af92e8ae1f27b7a1e6f478492a6f48fd98b71b8d2ef436c713fd3da904924b6f
661a42d0ac7fd9eb76e924a46e5fae3d564c0d30f9b9482dcc715291d9bc27ca
c1ccc2c(c1)OCO2
Br-[C;H0;D4;+0:1](-Br)(-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9].[OH;D1;+0:10]-[c:11](:[c:12]):[c:13](-[OH;D1;+0:14]):[c:15]>>[C:9]-[#8:8]-[C:6](=[O;D1;H0:7])-[C;H0;D4;+0:1]1(-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5])-[O;H0;D2;+0:10]-[c:11](:[c:12]):[c:13](:[c:15])-[O;H0;D2;+0:14]-1
73.2
[{"value": 73.2, "product": "C(C)OC(=O)C1(OC2=C(O1)C=CC=C2)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Ex-1A: Catechol (2.2 g, 20 mmol) was dissolved in acetone. Diethyl dibromomalonate (7.0 g, 22 mmol) and potassium carbonate (2.76 g) were added, and the mixture was stirred at room temperature overnight. The solvent was removed under reduced pressure, and water was added to the residue. The residue was extracted with d...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Ester.Ester.Aromatic alcohol.Aromatic alcohol
Ester.Ester.Ether.Ether
null
c1ccc2c(c1)OCO2
c1ccc2c(c1)OCO2
HBr
CC(=O)C
null
8
CCOC(=O)C(Br)(Br)C(=O)OCC.Oc1ccccc1O>CC(=O)C>CCOC(=O)C1(C(=O)OCC)Oc2ccccc2O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ffe68f0513c241bd8c2d2a4b859c46bf
COc1cc(C=O)cc(Br)c1OC.OB(O)c1cccs1>>COc1cc(C=O)cc(-c2cccs2)c1OC
S1C(=CC=C1)B(O)O.BrC=1C(=C(C=C(C=O)C1)OC)OC>>COC=1C=C(C=O)C=C(C1OC)C=1SC=CC1
Br[c:9]1[cH:8][c:5]([CH:6]=[O:7])[cH:4][c:3]([O:2][CH3:1])[c:15]1[O:16][CH3:17].OB(O)[c:10]1[cH:11][cH:12][cH:13][s:14]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH:6]=[O:7])[cH:8][c:9](-[c:10]2[cH:11][cH:12][cH:13][s:14]2)[c:15]1[O:16][CH3:17]
COc1cc(C=O)cc(Br)c1OC.OB(O)c1cccs1
COc1cc(C=O)cc(-c2cccs2)c1OC
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([O-])([O-])=O.[Na+].[Na+]
COCCOC
C-C Coupling
Suzuki coupling with boronic acids
a9e750b5cb26673fc488a731642519fa5963d6a2e4d2eeb976470c7f17606def
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cccs2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6](-[#8:7]):[c:8].O-B(-O)-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1>>[#8:7]-[c:6](:[c:8]):[c;H0;D3;+0:1](-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1):[c:2]:[c:3]-[C:4]=[O;D1;H0:5]
91
[{"value": 90.0, "product": "COC=1C=C(C=O)C=C(C1OC)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.0, "product": "COC=1C=C(C=O)C=C(C1OC)C=1SC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-1D: A solution of 5-bromo-3,4-dimethoxybenzaldehyde (10.23 g, 41.7 mmol) in 359 mL of ethylene glycol dimethyl ether was purged with nitrogen gas for 30 min. The solution was treated with tetrakis(triphenylphosphine)palladium(0) (5.0 g, 4.3 mmol), thiophene-2-boronic acid (8.01 g, 62.6 mmol), and a solution of 2 N s...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
HBr.B
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([O-])([O-])=O.[Na+].[Na+].COCCOC
null
null
COc1cc(C=O)cc(Br)c1OC.OB(O)c1cccs1>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([O-])([O-])=O.[Na+].[Na+].COCCOC>COc1cc(C=O)cc(-c2cccs2)c1OC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c0e35e5b2743478c94c3b16684e200e4
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cc2ccccc2s1>>COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
O.S1C2=C(C=C1B(O)O)C=CC=C2.C([O-])([O-])=O.[Na+].[Na+].BrC=1C(=CC(=C(C=O)C1)OC)OC>>S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2
Br[c:8]1[c:5]([O:6][CH3:7])[cH:4][c:3]([O:2][CH3:1])[c:19]([CH:20]=[O:21])[cH:18]1.OB(O)[c:9]1[cH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[s:17]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[s:17]2)[cH:18][c:19]1[CH:20]=[O:21]
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cc2ccccc2s1
COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
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
COCCOC
C-C Coupling
Suzuki coupling with boronic acids
a1259a94b31ac9f1988cb839e0910c5b2437b7522341904299ff46277eacea87
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cc3ccccc3s2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6](-[#8:7]):[c:8].O-B(-O)-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1>>[#8:7]-[c:6](:[c:8]):[c;H0;D3;+0:1](-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1):[c:2]:[c:3]-[C:4]=[O;D1;H0:5]
83
[{"value": 83.0, "product": "S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.6, "product": "S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
Ex-3A: A sample of 5-bromo-2,4-dimethoxybenzaldehyde (4.9 g, 20.0 mmol) was dissolved in ethylene glycol dimethyl ether (50 mL). Tetrakis(triphenylphosphine)palladium(0) (2.32 g, 2 mmol) was added, and the mixture was stirred at room temperature under nitrogen for 5 min. Benzo[b]thiophene-2-boronic acid (4.27 g, 24 mmo...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccc2sccc2c1
c1ccccc1.c1ccc2sccc2c1
c1ccccc1.c1ccc2sccc2c1
HBr.B
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.COCCOC
null
0.083333
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cc2ccccc2s1>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.COCCOC>COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c42bc816958d46fdb487d1fa20a0e374
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cc2ccccc2s1>>COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
BrC=1C(=CC(=C(C=O)C1)OC)OC.S1C2=C(C=C1B(O)O)C=CC=C2>>S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2
Br[c:8]1[c:5]([O:6][CH3:7])[cH:4][c:3]([O:2][CH3:1])[c:19]([CH:20]=[O:21])[cH:18]1.OB(O)[c:9]1[cH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[s:17]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[s:17]2)[cH:18][c:19]1[CH:20]=[O:21]
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cc2ccccc2s1
COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
null
null
C1CCOC1
C-C Coupling
Suzuki coupling with boronic acids
a1259a94b31ac9f1988cb839e0910c5b2437b7522341904299ff46277eacea87
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cc3ccccc3s2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6](-[#8:7]):[c:8].O-B(-O)-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1>>[#8:7]-[c:6](:[c:8]):[c;H0;D3;+0:1](-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1):[c:2]:[c:3]-[C:4]=[O;D1;H0:5]
97.5
[{"value": 97.0, "product": "S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.5, "product": "S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
1.5
HOUR
An alternative procedure: 5-bromo-2,4-dimethoxybenzaldehyde (20 g), benzo[b]thiophene-2-boronic acid (16 g) and THF (200 mL) were sequentially charged into a clean reaction vessel fitted with a reflux condenser, mechanical stirrer and nitrogen inlet adapter. Nitrogen was bubbled into the resulting solution for 20 min f...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccc2sccc2c1
c1ccccc1.c1ccc2sccc2c1
c1ccccc1.c1ccc2sccc2c1
HBr.B
C1CCOC1
60
1.5
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cc2ccccc2s1>C1CCOC1>COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-80ec1d096bde430b80ffb02cef23687a
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O>>COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
C(C)(=O)C1=CC=C(C(=O)O)C=C1.S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2.[OH-].[Na+]>>S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C=CC=C2
[CH3:21][C:22](=[O:23])[c:24]1[cH:25][cH:26][c:27]([C:28](=[O:29])[OH:30])[cH:31][cH:32]1.O=[CH:20][c:19]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[s:17]2)[cH:18]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14...
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
null
null
O.CN(C=O)C
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cc3ccccc3s2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
54
[{"value": 54.0, "product": "S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a solution of 4-acetylbenzoic acid (1.50 g, 9.1 mmol) and 5-(benzo[b]thien-2-yl)-2,4-dimethoxybenzaldehyde from Ex-3A (3.27 g, 11.0 mmol) in N,N-dimethylformamide (76 mL) was added a solution of sodium hydroxide (5 M, 7.3 mL, 36.5 mmol). The reaction mixture was allowed to stir at room temperature for 2 h and was th...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccc2sccc2c1.c1ccccc1
HO-
O.CN(C=O)C
null
2
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O>O.CN(C=O)C>COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dbc0fbc72a9c45638282d8de69c914ca
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O>>COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
O([Li])C.S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2.C(C)(=O)C1=CC=C(C(=O)O)C=C1.CO>>S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C=CC=C2
[CH3:21][C:22](=[O:23])[c:24]1[cH:25][cH:26][c:27]([C:28](=[O:29])[OH:30])[cH:31][cH:32]1.O=[CH:20][c:19]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[s:17]2)[cH:18]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14...
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
null
null
CCCCCCC.O.CN(C)C=O
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cc3ccccc3s2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
87
[{"value": 87.0, "product": "S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
An alternative procedure: 5-(Benzo[b]thien-2-yl)-2,4-dimethoxybenzaldehyde from Ex-3A (42.3 g), 4-acetylbenzoic acid (22.1 g), MeOH (250 mL) and DMF (600 mL) were sequentially charged into a clean reaction vessel fitted with a mechanical stirrer and nitrogen inlet adapter. After complete dissolution, LiOMe (10.5 g) was...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccc2sccc2c1.c1ccccc1
HO-
CCCCCCC.O.CN(C)C=O
null
2
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O>CCCCCCC.O.CN(C)C=O>COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-910e529f4bf849c9af867aee4fa5dbc9
O=Cc1ccc(Br)cc1.OB(O)c1nccs1>>O=Cc1ccc(-c2nccs2)cc1
BrC1=CC=C(C=O)C=C1.S1C(=NC=C1)B(O)O>>S1C(=NC=C1)C1=CC=C(C=O)C=C1
Br[c:6]1[cH:5][cH:4][c:3]([CH:2]=[O:1])[cH:13][cH:12]1.OB(O)[c:7]1[n:8][cH:9][cH:10][s:11]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[n:8][cH:9][cH:10][s:11]2)[cH:12][cH:13]1
O=Cc1ccc(Br)cc1.OB(O)c1nccs1
O=Cc1ccc(-c2nccs2)cc1
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
f4565b4e9dabb73b09ab28617730b65da20c1e6e94d183a4606dbf1402c06c05
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2nccs2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6]1:[#16;a:7]:[c:8]:[c:9]:[#7;a:10]:1>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6]1:[#16;a:7]:[c:8]:[c:9]:[#7;a:10]:1):[c:4]:[c:5]
82
[{"value": 82.0, "product": "S1C(=NC=C1)C1=CC=C(C=O)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-5A: 4-Thiazol-2-yl-benzaldehyde was prepared from 4-bromobenzaldehyde and thiazole-2-boronic acid in a similar manner as described in Ex-3A, 82% yield. 1H-NMR (CDCl3) δ 10.07 (s, 1H), 8.15 (d, J=8 Hz, 2H), 7.95–7.98 (m, 3H), 7.45 (d, J=3 Hz, 1H). HMRS (EI) calcd. for C10H7NOS: 189.0248; found: 189.0242. Conditions: ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1cscn1
c1ccccc1.c1cscn1
c1ccccc1.c1cscn1
HBr.B
null
null
null
O=Cc1ccc(Br)cc1.OB(O)c1nccs1>>O=Cc1ccc(-c2nccs2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f16ab514fd824af09929b4295ce2adb4
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cccs1>>COc1cc(OC)c(-c2cccs2)cc1C=O
BrC=1C(=CC(=C(C=O)C1)OC)OC.S1C(=CC=C1)B(O)O>>COC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1
Br[c:8]1[c:5]([O:6][CH3:7])[cH:4][c:3]([O:2][CH3:1])[c:15]([CH:16]=[O:17])[cH:14]1.OB(O)[c:9]1[cH:10][cH:11][cH:12][s:13]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][cH:11][cH:12][s:13]2)[cH:14][c:15]1[CH:16]=[O:17]
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cccs1
COc1cc(OC)c(-c2cccs2)cc1C=O
null
null
C1CCOC1
C-C Coupling
Suzuki coupling with boronic acids
a9e750b5cb26673fc488a731642519fa5963d6a2e4d2eeb976470c7f17606def
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cccs2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6](-[#8:7]):[c:8].O-B(-O)-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1>>[#8:7]-[c:6](:[c:8]):[c;H0;D3;+0:1](-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1):[c:2]:[c:3]-[C:4]=[O;D1;H0:5]
94
[{"value": 94.0, "product": "COC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.9, "product": "COC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
null
null
Ex-6A: 5-bromo-2,4-dimethoxybenzaldehyde (20.3 g), thiophene-2-boronic acid (11.6 g) and THF (200 mL) were sequentially charged into a clean reaction vessel fitted with a reflux condenser, mechanical stirrer and nitrogen inlet adapter. Nitrogen was bubbled into the resulting solution for 20 min followed by the sequenti...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
HBr.B
C1CCOC1
60
null
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cccs1>C1CCOC1>COc1cc(OC)c(-c2cccs2)cc1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2cfd49376d34445eab0e8f2771463ec3
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cccs2)cc1C=O>>COc1cc(OC)c(-c2cccs2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
C(C)(C)OC(=O)C.COC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1.C(C)(=O)C1=CC=C(C(=O)O)C=C1.Cl.O([Li])C>>COC1=C(C=C(C(=C1)OC)C=1SC=CC1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1
[CH3:17][C:18](=[O:19])[c:20]1[cH:21][cH:22][c:23]([C:24](=[O:25])[OH:26])[cH:27][cH:28]1.O=[CH:16][c:15]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][cH:11][cH:12][s:13]2)[cH:14]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][cH:11][cH:12][s:13]2)[cH:14][c:15]1/[CH:16]=[CH:17]/[C...
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cccs2)cc1C=O
COc1cc(OC)c(-c2cccs2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
null
null
CO.O.CN(C)C=O
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cccs2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
75
[{"value": 75.0, "product": "COC1=C(C=C(C(=C1)OC)C=1SC=CC1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
2,4-Dimethoxy-5-thiophen-2-yl-benzaldehyde from Ex-6A (7.81 g), 4-acetylbenzoic acid (4.9 g), MeOH (60 mL) and DMF (150 mL) were sequentially charged into a clean reaction vessel fitted with a stir bar and nitrogen inlet adapter. After complete dissolution LiOMe (4.60 g) was added and the resulting solution was aged fo...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccsc1.c1ccccc1
HO-
CO.O.CN(C)C=O
null
5
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cccs2)cc1C=O>CO.O.CN(C)C=O>COc1cc(OC)c(-c2cccs2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-98c5286fa77743c5adb9e6a08b1dd3b4
CC(=O)c1ccc(Br)cc1.OB(O)c1cccs1>>CC(=O)c1ccc(-c2cccs2)cc1
BrC1=CC=C(C=C1)C(C)=O.S1C(=CC=C1)B(O)O.C([O-])([O-])=O.[Na+].[Na+]>>S1C(=CC=C1)C1=CC=C(C=C1)C(C)=O
Br[c:7]1[cH:6][cH:5][c:4]([C:2]([CH3:1])=[O:3])[cH:14][cH:13]1.OB(O)[c:8]1[cH:9][cH:10][cH:11][s:12]1>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7](-[c:8]2[cH:9][cH:10][cH:11][s:12]2)[cH:13][cH:14]1
CC(=O)c1ccc(Br)cc1.OB(O)c1cccs1
CC(=O)c1ccc(-c2cccs2)cc1
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
COCCOC
C-C Coupling
Suzuki coupling with boronic acids
a9e750b5cb26673fc488a731642519fa5963d6a2e4d2eeb976470c7f17606def
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cccs2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6]1:[#16;a:7]:[c:8]:[c:9]:[c:10]:1>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6]1:[#16;a:7]:[c:8]:[c:9]:[c:10]:1):[c:4]:[c:5]
95.2
[{"value": 95.0, "product": "S1C(=CC=C1)C1=CC=C(C=C1)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.2, "product": "S1C(=CC=C1)C1=CC=C(C=C1)C(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-17A: 4′-Bromoacetophenone (3.98 g, 20 mmol) was dissolved in ethylene glycol dimethyl ether and then the solution was degassed with nitrogen for 15 minutes. Tetrakis(triphenylphosphine)palladium(0) (2.31 g, 2 mmol) was added, and the solution was further degassed for 10 minutes. Thiophene-2-boronic acid (3.07 g, 24 ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
HBr.B
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.COCCOC
null
null
CC(=O)c1ccc(Br)cc1.OB(O)c1cccs1>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.COCCOC>CC(=O)c1ccc(-c2cccs2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e7d528ac61244a92ae77ef18a8dc8431
COc1cc(-c2cccs2)ccc1C(C)=O.O=Cc1ccc(C(=O)O)cc1>>COc1cc(-c2cccs2)ccc1C(=O)/C=C/c1ccc(C(=O)O)cc1
COC1=C(C=CC(=C1)C=1SC=CC1)C(C)=O.C(=O)(O)C1=CC=C(C=O)C=C1>>COC1=C(C=CC(=C1)C=1SC=CC1)C(/C=C/C1=CC=C(C(=O)O)C=C1)=O
[CH3:1][O:2][c:3]1[cH:4][c:5](-[c:6]2[cH:7][cH:8][cH:9][s:10]2)[cH:11][cH:12][c:13]1[C:14](=[O:15])[CH3:16].O=[CH:17][c:18]1[cH:19][cH:20][c:21]([C:22](=[O:23])[OH:24])[cH:25][cH:26]1>>[CH3:1][O:2][c:3]1[cH:4][c:5](-[c:6]2[cH:7][cH:8][cH:9][s:10]2)[cH:11][cH:12][c:13]1[C:14](=[O:15])/[CH:16]=[CH:17]/[c:18]1[cH:19][cH:2...
COc1cc(-c2cccs2)ccc1C(C)=O.O=Cc1ccc(C(=O)O)cc1
COc1cc(-c2cccs2)ccc1C(=O)/C=C/c1ccc(C(=O)O)cc1
null
null
null
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1ccccc1)c1ccc(-c2cccs2)cc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
The title compound was prepared by condensing 1-(2-methoxy-4-thiophen-2-yl-phenyl)-ethanone (Ex-19A) and 4-carboxybenzaldehyde in a similar manner as described in Ex-17 except an acidic workup. Yellow solid, mp 193–195° C. 1H-NMR (CDCl3) □ 7.70 (d, J=8 Hz, 2H), 7.38 (d, J=8 Hz, 1H), 7.07–7.16 (m, 4H), 6.75–6.80 (m, 4H)...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccsc1.c1ccccc1
HO-
null
null
null
COc1cc(-c2cccs2)ccc1C(C)=O.O=Cc1ccc(C(=O)O)cc1>>COc1cc(-c2cccs2)ccc1C(=O)/C=C/c1ccc(C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c5484a2773bb47e29713adbda40748dc
O=Cc1ccc(F)c(Br)c1.OB(O)c1cccs1>>O=Cc1ccc(F)c(-c2cccs2)c1
O.BrC=1C=C(C=O)C=CC1F.S1C(=CC=C1)B(O)O.C([O-])([O-])=O.[Na+].[Na+]>>FC1=C(C=C(C=O)C=C1)C=1SC=CC1
Br[c:8]1[c:6]([F:7])[cH:5][cH:4][c:3]([CH:2]=[O:1])[cH:14]1.OB(O)[c:9]1[cH:10][cH:11][cH:12][s:13]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([F:7])[c:8](-[c:9]2[cH:10][cH:11][cH:12][s:13]2)[cH:14]1
O=Cc1ccc(F)c(Br)c1.OB(O)c1cccs1
O=Cc1ccc(F)c(-c2cccs2)c1
null
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1
COCCOC
C-C Coupling
Suzuki coupling with boronic acids
a9e750b5cb26673fc488a731642519fa5963d6a2e4d2eeb976470c7f17606def
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cccs2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6](-[F;D1;H0:7]):[c:8].O-B(-O)-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1>>[F;D1;H0:7]-[c:6](:[c:8]):[c;H0;D3;+0:1](-[c;H0;D3;+0:9]1:[#16;a:10]:[c:11]:[c:12]:[c:13]:1):[c:2]:[c:3]-[C:4]=[O;D1;H0:5]
95
[{"value": 95.0, "product": "FC1=C(C=C(C=O)C=C1)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 94.6, "product": "FC1=C(C=C(C=O)C=C1)C=1SC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-20A: A solution of 3-bromo-4-flouro-benzaldehyde (5.0 g, 24.6 mmol) and thiophene-2-boronic acid (4.7 g, 37.0 mmol) in ethylene glycol dimethyl ether (100 mL) was stirred at room temperature under nitrogen for 15 min. Then tetrakis(triphenylphosphine)-palladium(0) (2.8 g, 2.42 mmol) and a sodium carbonate solution (...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
HBr.B
[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.COCCOC
null
null
O=Cc1ccc(F)c(Br)c1.OB(O)c1cccs1>[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.COCCOC>O=Cc1ccc(F)c(-c2cccs2)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b5f1fe8613fa4da4a8336dfb85be8fde
C1CCNC1.O=Cc1ccc(F)c(-c2cccs2)c1>>O=Cc1ccc(N2CCCC2)c(-c2cccs2)c1
O.FC1=C(C=C(C=O)C=C1)C=1SC=CC1.N1CCCC1.C(=O)([O-])[O-].[K+].[K+]>>N1(CCCC1)C1=C(C=C(C=O)C=C1)C=1SC=CC1
[NH:7]1[CH2:8][CH2:9][CH2:10][CH2:11]1.F[c:6]1[cH:5][cH:4][c:3]([CH:2]=[O:1])[cH:18][c:12]1-[c:13]1[cH:14][cH:15][cH:16][s:17]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]([N:7]2[CH2:8][CH2:9][CH2:10][CH2:11]2)[c:12](-[c:13]2[cH:14][cH:15][cH:16][s:17]2)[cH:18]1
C1CCNC1.O=Cc1ccc(F)c(-c2cccs2)c1
O=Cc1ccc(N2CCCC2)c(-c2cccs2)c1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation secondary amine
389dbc6c760ba22d5b089335787069e4da1dc4ed4889d745a0e1de1824c34c09
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1csc(-c2ccccc2N2CCCC2)c1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[c:5]:[#16;a:6]):[c:7].[C:8]1-[C:9]-[NH;D2;+0:10]-[C:11]-[C:12]-1>>[#16;a:6]:[c:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[N;H0;D3;+0:10]1-[C:9]-[C:8]-[C:12]-[C:11]-1):[c:2]:[c:3]
29
[{"value": 29.0, "product": "N1(CCCC1)C1=C(C=C(C=O)C=C1)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 28.9, "product": "N1(CCCC1)C1=C(C=C(C=O)C=C1)C=1SC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-20B: A solution of 4-fluoro-3-(thiophen-2-yl)-benzaldehyde (1.11 g, 5.38 mmol) from Ex-20A and pyrrolidine (13.0 g, 183.0 mmol) in dimethylformamide (30 mL) was treated with solid K2CO3 (1.7 g, 12.3 mmol), and the resulting mixture was stirred at reflux for 1 week. Upon cooling to room temperature, the reaction was ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CCNC1.c1ccccc1
c1ccccc1.C1CC[NH]C1
c1ccccc1.C1CC[NH]C1.c1ccsc1
HF
CN(C=O)C
null
null
C1CCNC1.O=Cc1ccc(F)c(-c2cccs2)c1>CN(C=O)C>O=Cc1ccc(N2CCCC2)c(-c2cccs2)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3710f1d466844c3a80b01c2a0dd8ec27
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(N2CCCC2)c(-c2cccs2)c1>>O=C(O)c1ccc(C(=O)/C=C/c2ccc(N3CCCC3)c(-c3cccs3)c2)cc1
N1(CCCC1)C1=C(C=C(C=O)C=C1)C=1SC=CC1.C(C)(=O)C1=CC=C(C(=O)O)C=C1.[OH-].[Na+]>>N1(CCCC1)C1=C(C=C(C=C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)C=1SC=CC1
[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]([C:8](=[O:9])[CH3:10])[cH:28][cH:29]1.O=[CH:11][c:12]1[cH:13][cH:14][c:15]([N:16]2[CH2:17][CH2:18][CH2:19][CH2:20]2)[c:21](-[c:22]2[cH:23][cH:24][cH:25][s:26]2)[cH:27]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]([C:8](=[O:9])/[CH:10]=[CH:11]/[c:12]2[cH:13][cH:14][c:15]([N:16]...
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(N2CCCC2)c(-c2cccs2)c1
O=C(O)c1ccc(C(=O)/C=C/c2ccc(N3CCCC3)c(-c3cccs3)c2)cc1
null
null
O.CN(C=O)C
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1ccc(N2CCCC2)c(-c2cccs2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
13
[{"value": 13.0, "product": "N1(CCCC1)C1=C(C=C(C=C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 12.8, "product": "N1(CCCC1)C1=C(C=C(C=C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)C=1SC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
4-Pyrrolidin-1-yl-3-(thiophen-2-yl)-benzaldehyde (400 mg, 1.55 mmol) from Ex-20B and 4-acetylbenzoic acid (255 mg, 1.55 mmol) were dissolved in dimethylformamide (30 mL). Sodium hydroxide solution (5 N, 1.25 mL) was added in one portion, and the mixture was stirred at room temperature overnight. The reaction was dilute...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccccc1.C1CC[NH]C1.c1ccsc1
HO-
O.CN(C=O)C
null
8
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(N2CCCC2)c(-c2cccs2)c1>O.CN(C=O)C>O=C(O)c1ccc(C(=O)/C=C/c2ccc(N3CCCC3)c(-c3cccs3)c2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2a580c9cc4a04d5ca1251353720da926
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(F)c(-c2cccs2)c1>>O=C(O)c1ccc(C(=O)/C=C/c2ccc(F)c(-c3cccs3)c2)cc1
FC1=C(C=C(C=O)C=C1)C=1SC=CC1.C(C)(=O)C1=CC=C(C(=O)O)C=C1.[OH-].[Na+]>>FC1=C(C=C(C=C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)C=1SC=CC1
[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]([C:8](=[O:9])[CH3:10])[cH:24][cH:25]1.O=[CH:11][c:12]1[cH:13][cH:14][c:15]([F:16])[c:17](-[c:18]2[cH:19][cH:20][cH:21][s:22]2)[cH:23]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]([C:8](=[O:9])/[CH:10]=[CH:11]/[c:12]2[cH:13][cH:14][c:15]([F:16])[c:17](-[c:18]3[cH:19][cH:20][cH:...
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(F)c(-c2cccs2)c1
O=C(O)c1ccc(C(=O)/C=C/c2ccc(F)c(-c3cccs3)c2)cc1
null
null
O.CN(C=O)C
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cccs2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
53
[{"value": 53.0, "product": "FC1=C(C=C(C=C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 52.7, "product": "FC1=C(C=C(C=C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)C=1SC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
4-Fluoro-3-thiophen-2-yl-benzaldehyde (1.0 g, 4.85 mmol, from Ex-20A) and 4-acetylbenzoic acid (0.80 g, 4.87 mmol) were dissolved in dimethylformamide (55 mL). Sodium hydroxide solution (5 N, 3.88 mL) was added in one portion, and the mixture was stirred at room temperature for 3 h. The reaction was diluted with water ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccccc1.c1ccsc1
HO-
O.CN(C=O)C
null
3
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(F)c(-c2cccs2)c1>O.CN(C=O)C>O=C(O)c1ccc(C(=O)/C=C/c2ccc(F)c(-c3cccs3)c2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6dfae3c96f5446508413bd94bf9d0b34
CC(=O)c1ccc(SCC(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O>>COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(SCC(=O)O)cc1
C(C)(=O)C1=CC=C(C=C1)SCC(=O)O.S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2>>S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C=C1)SCC(=O)O)OC)OC)C=CC=C2
[CH3:21][C:22](=[O:23])[c:24]1[cH:25][cH:26][c:27]([S:28][CH2:29][C:30](=[O:31])[OH:32])[cH:33][cH:34]1.O=[CH:20][c:19]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[s:17]2)[cH:18]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12...
CC(=O)c1ccc(SCC(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(SCC(=O)O)cc1
null
null
null
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cc3ccccc3s2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
The title compound was prepared by condensing (4-acetylphenylthio)acetic acid (Ex-23B) and 5-(benzo[b]thien-2-yl)-2,4-dimethoxybenzaldehyde (Ex-3A) in a similar manner as described in Ex-22. Yellow solid, mp 136–138° C. (dec.). 1H-NMR (DMSO-d6) δ 8.35 (s, 1H), 8.08 (d, J=7.4 Hz, 2H), 8.03 (d, J=16.3 Hz, 1H), 7.93–7.87 ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccc2sccc2c1.c1ccccc1
HO-
null
null
null
CC(=O)c1ccc(SCC(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O>>COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(SCC(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-df59b97702e6473b8f3c2590b665ace4
CC(=O)c1ccc(S(=O)(=O)Cl)cc1.N>>CC(=O)c1ccc(S(N)(=O)=O)cc1
C(C)(=O)C1=CC=C(C=C1)S(=O)(=O)Cl.N>>C(C)(=O)C1=CC=C(C=C1)S(=O)(=O)N
Cl[S:8]([c:7]1[cH:6][cH:5][c:4]([C:2]([CH3:1])=[O:3])[cH:13][cH:12]1)(=[O:10])=[O:11].[NH3:9]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]([S:8]([NH2:9])(=[O:10])=[O:11])[cH:12][cH:13]1
CC(=O)c1ccc(S(=O)(=O)Cl)cc1.N
CC(=O)c1ccc(S(N)(=O)=O)cc1
null
null
CC(=O)C
Acylation
OtherReaction
672a14b4f1ef0b966898e1b4c118f241f21df1d6e087372155b9d0c840dac61f
29e1633db8f1f00444181a0bcac91d574ed806fddf9165be4c8478fc32a80994
c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[NH3;D0;+0:7]>>[NH2;D1;+0:7]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
93
[{"value": 93.0, "product": "C(C)(=O)C1=CC=C(C=C1)S(=O)(=O)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.0, "product": "C(C)(=O)C1=CC=C(C=C1)S(=O)(=O)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
Ex-26A: To a solution of 4-acetyl-benzenesulfonyl chloride (Hoffman, R. V. Org. Syn. VII, 508; 4.18 g, 19.1 mmol) in acetone (30 mL) was added ammonia (28% in water, 8.2 mL, 57.3 mmol) dropwise at 0° C. The reaction mixture was allowed to stir at 0° C. for 30 min. The precipitate was filtered and the residue was washed...
10.6084/m9.figshare.5104873.v1
null
Sulfonyl halide
Sulfonamide
null
null
c1ccccc1
HCl
CC(=O)C
0
0.5
CC(=O)c1ccc(S(=O)(=O)Cl)cc1.N>CC(=O)C>CC(=O)c1ccc(S(N)(=O)=O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9ccfd343f2824477a48c1ff905b1543b
CC(=O)c1ccc2[nH]ccc2c1.CI>>CC(=O)c1ccc2c(ccn2C)c1
IC.N1C=CC2=CC(=CC=C12)C(C)=O.IC.C([O-])([O-])=O.[Cs+].[Cs+]>>CN1C=CC2=CC(=CC=C12)C(C)=O
[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]2[c:8]([cH:9][cH:10][nH:11]2)[cH:13]1.I[CH3:12]>>[CH3:1][C:2](=[O:3])[c:4]1[cH:5][cH:6][c:7]2[c:8]([cH:9][cH:10][n:11]2[CH3:12])[cH:13]1
CC(=O)c1ccc2[nH]ccc2c1.CI
CC(=O)c1ccc2c(ccn2C)c1
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
5f4295751cbf2eac77c77b599ebb727e1800dd106de3a7476670f0ac76dbeba5
7a358c636daddc97c1fb4c29f378044d7eac3f01815d9966e599841f642d631a
c1ccc2[nH]ccc2c1
I-[CH3;D1;+0:1].[c:2]:[c:3]1:[c:4]:[c:5]:[c:6]:[nH;D2;+0:7]:1>>[CH3;D1;+0:1]-[n;H0;D3;+0:7]1:[c:6]:[c:5]:[c:4]:[c:3]:1:[c:2]
51.5
[{"value": 51.0, "product": "CN1C=CC2=CC(=CC=C12)C(C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 51.5, "product": "CN1C=CC2=CC(=CC=C12)C(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-28A: To a solution of 1-(1H-indol-5-yl)-ethanone (Yang, Y. et al, Heterocycles, 1992, 34(6), 1169–1175; 0.45 g, 2.8 mmol) were added iodomethane (3 mL) and cesium carbonate (2.3 g, 7.1 mmol). The reaction mixture was allowed to stir at 55° C. for 1.5 day during which additional iodomethane (11 mL) was added. The rea...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
c1ccc2[nH]ccc2c1
HI
null
null
null
CC(=O)c1ccc2[nH]ccc2c1.CI>>CC(=O)c1ccc2c(ccn2C)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-361e00b4c4e24068ba682d59610004f6
BrBr.COc1ccc(C=O)c(O)c1>>COc1cc(O)c(C=O)cc1Br
OC1=C(C=O)C=CC(=C1)OC.BrBr>>BrC=1C(=CC(=C(C=O)C1)O)OC
Br[Br:12].[CH3:1][O:2][c:3]1[cH:4][c:5]([OH:6])[c:7]([CH:8]=[O:9])[cH:10][cH:11]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([OH:6])[c:7]([CH:8]=[O:9])[cH:10][c:11]1[Br:12]
BrBr.COc1ccc(C=O)c(O)c1
COc1cc(O)c(C=O)cc1Br
null
null
ClCCl
Functional Group Interconversion
Bromination
f6effe61353895b318215d8bd9b6bb1105cafbf7be8c217d748df587260b32c3
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccccc1
Br-[Br;H0;D1;+0:1].[#8:2]-[c:3](:[c:4]):[cH;D2;+0:5]:[c:6]:[c:7]-[C:8]=[O;D1;H0:9]>>[#8:2]-[c:3](:[c:4]):[c;H0;D3;+0:5](-[Br;H0;D1;+0:1]):[c:6]:[c:7]-[C:8]=[O;D1;H0:9]
80
[{"value": 80.0, "product": "BrC=1C(=CC(=C(C=O)C1)O)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.8, "product": "BrC=1C(=CC(=C(C=O)C1)O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
Ex-29A: 2-Hydroxy-4-methoxybenzaldehyde (6.0 g, 39 mmol) was dissolved in dichloromethane (50 mL) and cooled to 0° C. using an ice-water bath. Bromine (6.8 g, 43 mmol) in dichloromethane (2 mL) was added dropwise to the cooled solution and stirred for 2 h at 0° C. The mixture was warmed to room temperature and stirred ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccccc1
c1ccccc1
c1ccccc1
HBr
ClCCl
0
2
BrBr.COc1ccc(C=O)c(O)c1>ClCCl>COc1cc(O)c(C=O)cc1Br
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-07e91bbb9f5246f988cf42bf69e03215
COCCOCCBr.COc1cc(O)c(C=O)cc1-c1cccs1>>COCCOCCOc1cc(OC)c(-c2cccs2)cc1C=O
BrCCOCCOC.OC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1.C([O-])([O-])=O.[K+].[K+]>>COC1=CC(=C(C=O)C=C1C=1SC=CC1)OCCOCCOC
Br[CH2:7][CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1].[OH:8][c:9]1[cH:10][c:11]([O:12][CH3:13])[c:14](-[c:15]2[cH:16][cH:17][cH:18][s:19]2)[cH:20][c:21]1[CH:22]=[O:23]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][O:8][c:9]1[cH:10][c:11]([O:12][CH3:13])[c:14](-[c:15]2[cH:16][cH:17][cH:18][s:19]2)[cH:20][c:21]1[CH:22]=[O:23]
COCCOCCBr.COc1cc(O)c(C=O)cc1-c1cccs1
COCCOCCOc1cc(OC)c(-c2cccs2)cc1C=O
null
null
O.CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ccc(-c2cccs2)cc1
Br-[CH2;D2;+0:1]-[C:2]-[#8:3].[O;D1;H0:4]=[C:5]-[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:8]-[c:7](:[c:9]):[c:6]-[C:5]=[O;D1;H0:4]
87
[{"value": 87.0, "product": "COC1=CC(=C(C=O)C=C1C=1SC=CC1)OCCOCCOC", "details": "PERCENTYIELD", "is_desired": false}]
80
CELSIUS
1
HOUR
Ex-29C: To a solution of 2-hydroxy-4-methoxy-5-thiophen-2-yl-benzaldehyde from Ex-29B (0.10 g, 0.43 mmol) in N,N-dimethylformamide (3 mL) was added potassium carbonate (0.18 g, 1.3 mmol) and the resulting yellow slurry was heated to 80° C. Once at 80° C., 1-bromo-2-(2-methoxyethoxy)ethane (0.24 g, 1.3 mmol) was added d...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1.c1ccsc1
HBr
O.CN(C=O)C
80
1
COCCOCCBr.COc1cc(O)c(C=O)cc1-c1cccs1>O.CN(C=O)C>COCCOCCOc1cc(OC)c(-c2cccs2)cc1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8fc2ef8a042a46f58b067fa79d0eba07
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(-c2cccs2)cc1F>>O=C(O)c1ccc(C(=O)/C=C/c2ccc(-c3cccs3)cc2F)cc1
FC1=C(C=O)C=CC(=C1)C=1SC=CC1.C(C)(=O)C1=CC=C(C(=O)O)C=C1>>FC1=C(C=CC(=C1)C=1SC=CC1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1
[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]([C:8](=[O:9])[CH3:10])[cH:24][cH:25]1.O=[CH:11][c:12]1[cH:13][cH:14][c:15](-[c:16]2[cH:17][cH:18][cH:19][s:20]2)[cH:21][c:22]1[F:23]>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]([C:8](=[O:9])/[CH:10]=[CH:11]/[c:12]2[cH:13][cH:14][c:15](-[c:16]3[cH:17][cH:18][cH:19][s:20]3)[cH:2...
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(-c2cccs2)cc1F
O=C(O)c1ccc(C(=O)/C=C/c2ccc(-c3cccs3)cc2F)cc1
null
null
null
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1ccc(-c2cccs2)cc1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
71
[{"value": 71.0, "product": "FC1=C(C=CC(=C1)C=1SC=CC1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared by condensing 2-fluoro-4-thiophen-2-yl-benzaldehyde (Ex-30A) and 4-acetylbezoic acid in a similar manner as described in Ex-3. Yellow solid, 71% yield, m.p.>260° C. 1H-NMR (300 MHz, d6-DMSO): 8.19 (d, 2H, J=8.4 Hz), 8.12 (d, 1H, J=8 Hz), 8.06 (d, 2H, J=8 Hz), 7.95 (d, 1H, J=16 Hz), 7.80 ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccccc1.c1ccsc1
HO-
null
null
null
CC(=O)c1ccc(C(=O)O)cc1.O=Cc1ccc(-c2cccs2)cc1F>>O=C(O)c1ccc(C(=O)/C=C/c2ccc(-c3cccs3)cc2F)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a1360300cdb744508e0514350ce69833
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cncnc1>>COc1cc(OC)c(-c2cncnc2)cc1C=O
BrC=1C(=CC(=C(C=O)C1)OC)OC.N1=CN=CC(=C1)B(O)O>>COC1=C(C=O)C=C(C(=C1)OC)C=1C=NC=NC1
Br[c:8]1[c:5]([O:6][CH3:7])[cH:4][c:3]([O:2][CH3:1])[c:16]([CH:17]=[O:18])[cH:15]1.OB(O)[c:9]1[cH:10][n:11][cH:12][n:13][cH:14]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][n:11][cH:12][n:13][cH:14]2)[cH:15][c:16]1[CH:17]=[O:18]
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cncnc1
COc1cc(OC)c(-c2cncnc2)cc1C=O
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
5efc69cb0f56c6c241a71b9df28c03b094ed8fc2f31567997f12f88c03083478
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cncnc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6](-[#8:7]):[c:8].O-B(-O)-[c;H0;D3;+0:9]1:[c:10]:[#7;a:11]:[c:12]:[#7;a:13]:[c:14]:1>>[#8:7]-[c:6](:[c:8]):[c;H0;D3;+0:1](-[c;H0;D3;+0:9]1:[c:10]:[#7;a:11]:[c:12]:[#7;a:13]:[c:14]:1):[c:2]:[c:3]-[C:4]=[O;D1;H0:5]
98
[{"value": 98.0, "product": "COC1=C(C=O)C=C(C(=C1)OC)C=1C=NC=NC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-31A: 2,4-Dimethoxy-5-pyrimidin-5-yl-benzaldehyde was prepared from 5-bromo-2,4-dimethoxybenzaldehyde and pyrimidine-5-boronic acid in a similar manner as described in Ex-3A, 98% yield. 1H-NMR (CDCl3) δ 10.37 (s, 1H), 9.15 (s, 1H), 8.87 (s, 2H) 7.86 (s, 1H), 6.57 (s, 1H), 4.03 (s, 3H), 3.96 (s, 3H). Conditions: See r...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1cncnc1
c1ccccc1.c1cncnc1
c1ccccc1.c1cncnc1
HBr.B
null
null
null
COc1cc(OC)c(C=O)cc1Br.OB(O)c1cncnc1>>COc1cc(OC)c(-c2cncnc2)cc1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9c3dc3b392cd4438ba117a73b6f01262
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cncnc2)cc1C=O>>COc1cc(OC)c(-c2cncnc2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
COC1=C(C=O)C=C(C(=C1)OC)C=1C=NC=NC1.C(C)(=O)C1=CC=C(C(=O)O)C=C1>>COC1=C(C=C(C(=C1)OC)C=1C=NC=NC1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1
[CH3:18][C:19](=[O:20])[c:21]1[cH:22][cH:23][c:24]([C:25](=[O:26])[OH:27])[cH:28][cH:29]1.O=[CH:17][c:16]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][n:11][cH:12][n:13][cH:14]2)[cH:15]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][n:11][cH:12][n:13][cH:14]2)[cH:15][c:16]1/[CH:17...
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cncnc2)cc1C=O
COc1cc(OC)c(-c2cncnc2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
null
null
null
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cncnc2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
26
[{"value": 26.0, "product": "COC1=C(C=C(C(=C1)OC)C=1C=NC=NC1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared by condensing 2,4-dimethoxy-5-pyrimidin-5-yl-benzaldehyde (Ex-31A) and 4-acetylbezoic acid in a similar manner as described in Ex-3. Yellow solid, mp>260° C., 26% yield. 1H-NMR (DMSO-d6) δ 9.11 (s, 1H), 8.96 (s, 2H), 8.13–8.16 (m, 3H), 8.01–8.09 (m, 3H), 7.90 (d, J=15 Hz, 1H), 6.85 (s, 1...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1cncnc1.c1ccccc1
HO-
null
null
null
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cncnc2)cc1C=O>>COc1cc(OC)c(-c2cncnc2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2599c5c31bb8412fa660fff33be023f4
COc1cc(O)c(C=O)cc1-c1cccs1.ClCC1CC1>>COc1cc(OCC2CC2)c(C=O)cc1-c1cccs1
OC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1.ClCC1CC1>>C1(CC1)COC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1
[CH3:1][O:2][c:3]1[cH:4][c:5]([OH:6])[c:11]([CH:12]=[O:13])[cH:14][c:15]1-[c:16]1[cH:17][cH:18][cH:19][s:20]1.Cl[CH2:7][CH:8]1[CH2:9][CH2:10]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH2:7][CH:8]2[CH2:9][CH2:10]2)[c:11]([CH:12]=[O:13])[cH:14][c:15]1-[c:16]1[cH:17][cH:18][cH:19][s:20]1
COc1cc(O)c(C=O)cc1-c1cccs1.ClCC1CC1
COc1cc(OCC2CC2)c(C=O)cc1-c1cccs1
null
null
null
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1csc(-c2ccc(OCC3CC3)cc2)c1
Cl-[CH2;D2;+0:1]-[C:2]1-[C:3]-[C:4]-1.[O;D1;H0:5]=[C:6]-[c:7]:[c:8](-[OH;D1;+0:9]):[c:10]>>[O;D1;H0:5]=[C:6]-[c:7]:[c:8](-[O;H0;D2;+0:9]-[CH2;D2;+0:1]-[C:2]1-[C:3]-[C:4]-1):[c:10]
18
[{"value": 18.0, "product": "C1(CC1)COC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-32A: 2-Cyclopropylmethoxy-4-methoxy-5-thiophen-2-yl-benzaldehyde was prepared in a similar manner as described in Ex-29C from 2-hydroxy-4-methoxy-5-thiophen-2-yl-benzaldehyde (Ex. 29B) and chloromethyl-cyclopropane, 18% yield. 1H-NMR (CDCl3) δ 10.41 (s, 1H), 8.24 (s, 1H), 7.43 (d, 1H), 7.29 (d, 1H), 7.06 (t, 1H), 6....
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1.C1CC1.c1ccsc1
HCl
null
null
null
COc1cc(O)c(C=O)cc1-c1cccs1.ClCC1CC1>>COc1cc(OCC2CC2)c(C=O)cc1-c1cccs1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b93dc0ceba4e440a99747de054e06a40
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OCC2CC2)c(C=O)cc1-c1cccs1>>COc1cc(OCC2CC2)c(/C=C/C(=O)c2ccc(C(=O)O)cc2)cc1-c1cccs1
C1(CC1)COC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1.C(C)(=O)C1=CC=C(C(=O)O)C=C1>>C1(CC1)COC1=C(C=C(C(=C1)OC)C=1SC=CC1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1
[CH3:13][C:14](=[O:15])[c:16]1[cH:17][cH:18][c:19]([C:20](=[O:21])[OH:22])[cH:23][cH:24]1.O=[CH:12][c:11]1[c:5]([O:6][CH2:7][CH:8]2[CH2:9][CH2:10]2)[cH:4][c:3]([O:2][CH3:1])[c:26](-[c:27]2[cH:28][cH:29][cH:30][s:31]2)[cH:25]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH2:7][CH:8]2[CH2:9][CH2:10]2)[c:11](/[CH:12]=[CH:13]/[C:...
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OCC2CC2)c(C=O)cc1-c1cccs1
COc1cc(OCC2CC2)c(/C=C/C(=O)c2ccc(C(=O)O)cc2)cc1-c1cccs1
null
null
null
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cc(-c2cccs2)ccc1OCC1CC1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
The title compound was prepared by condensing 2-cyclopropylmethoxy-4-methoxy-5-thiophen-2-yl-benzaldehyde (Ex-32B) and 4-acetylbenzoic acid in a similar manner as described in Ex-3. Yellow solid, mp 187–191° C. 1H-NMR (DMSO-d6) δ 8.22 (d, 2H), 8.19 (s, 1H), 7.01 (m, 4H), 7.62 (d, 1H), 7.47 (d, 1H), 7.09 (t, 1H), 6.76 (...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.C1CC1.c1ccccc1.c1ccsc1
HO-
null
null
null
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OCC2CC2)c(C=O)cc1-c1cccs1>>COc1cc(OCC2CC2)c(/C=C/C(=O)c2ccc(C(=O)O)cc2)cc1-c1cccs1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cae727d29c5142bab06a1ae4493a7906
COc1cc(OC)c(C=O)cc1Br.Cc1noc(C)c1B(O)O>>COc1cc(OC)c(-c2c(C)noc2C)cc1C=O
BrC=1C(=CC(=C(C=O)C1)OC)OC.CC1=NOC(=C1B(O)O)C>>CC1=NOC(=C1C=1C(=CC(=C(C=O)C1)OC)OC)C
Br[c:8]1[c:5]([O:6][CH3:7])[cH:4][c:3]([O:2][CH3:1])[c:17]([CH:18]=[O:19])[cH:16]1.OB(O)[c:9]1[c:10]([CH3:11])[n:12][o:13][c:14]1[CH3:15]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[c:10]([CH3:11])[n:12][o:13][c:14]2[CH3:15])[cH:16][c:17]1[CH:18]=[O:19]
COc1cc(OC)c(C=O)cc1Br.Cc1noc(C)c1B(O)O
COc1cc(OC)c(-c2c(C)noc2C)cc1C=O
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
5b7dd82949a962746098cf241492f164306faeffdc0ae0e0292301e001a6c22c
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cnoc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6](-[#8:7]):[c:8].O-B(-O)-[c;H0;D3;+0:9]1:[c:10](-[C;D1;H3:11]):[#7;a:12]:[#8;a:13]:[c:14]:1-[C;D1;H3:15]>>[#8:7]-[c:6](:[c:8]):[c;H0;D3;+0:1](-[c;H0;D3;+0:9]1:[c:10](-[C;D1;H3:11]):[#7;a:12]:[#8;a:13]:[c:14]:1-[C;D1;H3:15]):[c:2]:[c:3]-[C:4]=[O;D1;H0:5]
75
[{"value": 75.0, "product": "CC1=NOC(=C1C=1C(=CC(=C(C=O)C1)OC)OC)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Ex-33A: 5-(3,5-Dimethyl-isoxazol-4-yl)-2,4-dimethoxy-benzaldehyde was prepared from 5-bromo-2,4-dimethoxybenzaldehyde and 3,5-dimethyl-isoxazole-4-boronic acid in a similar manner as described in Ex-3A, 75% yield. 1H-NMR (CDCl3) δ 10.34 (s, 1H), 7.63 (s, 1H), 6.52 (s, 1H), 4.00 (s, 3H), 3.90 (s, 3H), 2.12 (s, 6H). Cond...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1cnoc1
c1ccccc1.c1cnoc1
c1ccccc1.c1cnoc1
HBr.B
null
null
null
COc1cc(OC)c(C=O)cc1Br.Cc1noc(C)c1B(O)O>>COc1cc(OC)c(-c2c(C)noc2C)cc1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bf5538abf09f4116b115afb71cb81295
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2c(C)noc2C)cc1C=O>>COc1cc(OC)c(-c2c(C)noc2C)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
CC1=NOC(=C1C=1C(=CC(=C(C=O)C1)OC)OC)C.C(C)(=O)C1=CC=C(C(=O)O)C=C1>>CC1=NOC(=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C
[CH3:19][C:20](=[O:21])[c:22]1[cH:23][cH:24][c:25]([C:26](=[O:27])[OH:28])[cH:29][cH:30]1.O=[CH:18][c:17]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[c:10]([CH3:11])[n:12][o:13][c:14]2[CH3:15])[cH:16]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[c:10]([CH3:11])[n:12][o:13][c:14]2[CH3:15])[cH...
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2c(C)noc2C)cc1C=O
COc1cc(OC)c(-c2c(C)noc2C)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
null
null
null
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cnoc2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
7
[{"value": 7.0, "product": "CC1=NOC(=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared by condensing 5-(3,5-dimethyl-isoxazol-4-yl)-2,4-dimethoxy-benzaldehyde (Ex-33A) and 4-acetylbenzoic acid in a similar manner as described in Ex-3. Yellow solid, mp>260° C., 7% yield. 1H-NMR (DMSO-d6) δ 8.15 (d, J=8 Hz, 2H), 8.04 (d, J=16 Hz, 1H), 8.02 (d, J=8 Hz, 2H), 7.89 (s, 1H), 7.81...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1cnoc1.c1ccccc1
HO-
null
null
null
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2c(C)noc2C)cc1C=O>>COc1cc(OC)c(-c2c(C)noc2C)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8369248867f0408eb05df10e2fc0ea3b
COc1ccc(C=O)c(OS(=O)(=O)C(F)(F)F)c1.OB(O)c1cccs1>>COc1ccc(C=O)c(-c2cccs2)c1
S1C(=CC=C1)B(O)O.P(=O)([O-])([O-])[O-].[K+].[K+].[K+].C(=O)C1=C(C=C(C=C1)OC)OS(=O)(=O)C(F)(F)F>>COC1=CC(=C(C=O)C=C1)C=1SC=CC1
O=S(=O)(O[c:9]1[c:6]([CH:7]=[O:8])[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:15]1)C(F)(F)F.OB(O)[c:10]1[cH:11][cH:12][cH:13][s:14]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH:7]=[O:8])[c:9](-[c:10]2[cH:11][cH:12][cH:13][s:14]2)[cH:15]1
COc1ccc(C=O)c(OS(=O)(=O)C(F)(F)F)c1.OB(O)c1cccs1
COc1ccc(C=O)c(-c2cccs2)c1
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
CCOC(=O)C.O.O1CCOCC1
C-C Coupling
Suzuki coupling with boronic acids OTf
c69a6f6be1d8ce542404db514bc9846ba00a86118103061e95d9f239037a465f
3f602cf53fbcf2a56d992979503f6bea55727095a6b9075475a711784170b440
c1ccc(-c2cccs2)cc1
F-C(-F)(-F)-S(=O)(=O)-O-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]=[O;D1;H0:6]):[c:7].O-B(-O)-[c;H0;D3;+0:8]1:[#16;a:9]:[c:10]:[c:11]:[c:12]:1>>[O;D1;H0:6]=[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[c;H0;D3;+0:8]1:[#16;a:9]:[c:10]:[c:11]:[c:12]:1):[c:2]:[c:3]
90
[{"value": 90.0, "product": "COC1=CC(=C(C=O)C=C1)C=1SC=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.5, "product": "COC1=CC(=C(C=O)C=C1)C=1SC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
95
CELSIUS
null
null
Ex-34B: A solution of trifluoro-methanesulfonic acid 2-formyl-5-methoxy-phenyl ester (Ex-34A, 1.6 g, 5.63 mmol) in 1,4-dioxane (15 mL) was stirred at room temperature under nitrogen for 5 min. Thiophene-2-boronic acid (1.08 g, 8.44 mmol), tetrakis(triphenylphosphine)palladium(0) (0.65 g, 0.56 mmol) and a potassium phos...
10.6084/m9.figshare.5104873.v1
null
Triflate.Boronic acid
null
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
c1ccccc1.c1ccsc1
TfOH.HO-.B
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.CCOC(=O)C.O.O1CCOCC1
95
null
COc1ccc(C=O)c(OS(=O)(=O)C(F)(F)F)c1.OB(O)c1cccs1>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.CCOC(=O)C.O.O1CCOCC1>COc1ccc(C=O)c(-c2cccs2)c1