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-018fd0e1351f4fd09b20fcddd97b4c7a
ord-73007926fa184342830a1dbd65d16aa0
COC(=O)Cc1ccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)cc1>>Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3ccc(CC(=O)O)cc3)nc21
ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC2=CC=C(C=C2)CC(=O)OC)N(C1=O)C.[OH-].[Na+].C(C)(=O)O>>ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC2=CC=C(C=C2)CC(=O)O)N(C1=O)C
C[O:27][C:25]([CH2:24][c:23]1[cH:22][cH:21][c:20]([NH:19][c:18]2[n:17][cH:16][c:15]3[cH:14][c:5](-[c:6]4[c:7]([Cl:8])[cH:9][cH:10][cH:11][c:12]4[Cl:13])[c:3](=[O:4])[n:2]([CH3:1])[c:31]3[n:30]2)[cH:29][cH:28]1)=[O:26]>>[CH3:1][n:2]1[c:3](=[O:4])[c:5](-[c:6]2[c:7]([Cl:8])[cH:9][cH:10][cH:11][c:12]2[Cl:13])[cH:14][c:15]2...
COC(=O)Cc1ccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)cc1
Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3ccc(CC(=O)O)cc3)nc21
null
null
CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1ccccc1
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
A quantity of 0.065 g (0.14 mmol) of {4-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino]phenyl}-acetic acid, methyl ester of Example 84 was dissolved in 25 mL of hot methanol with stirring. At the boiling point, 1 mL of 2N sodium hydroxide was added. After 1 hour reflux, the solution...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1cnc2ncncc2c1.c1ccccc1
Other
CO
null
null
COC(=O)Cc1ccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)cc1>CO>Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3ccc(CC(=O)O)cc3)nc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9fd5cd2b22e5454fb149f6f3ed738293
CCOC(=O)c1cccc(N)c1.Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(S(C)(=O)=O)nc21>>CCOC(=O)c1cccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)c1
ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)S(=O)(=O)C)N(C1=O)C.NC=1C=C(C(=O)OCC)C=CC1.C(C)(=O)O>>ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC=2C=C(C(=O)OCC)C=CC2)N(C1=O)C
[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][cH:9][c:10]([NH2:11])[cH:32]1.CS(=O)(=O)[c:12]1[n:13][cH:14][c:15]2[cH:16][c:17](-[c:18]3[c:19]([Cl:20])[cH:21][cH:22][cH:23][c:24]3[Cl:25])[c:26](=[O:27])[n:28]([CH3:29])[c:30]2[n:31]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][cH:9][c:10]([NH:11][c:12]2[n:13...
CCOC(=O)c1cccc(N)c1.Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(S(C)(=O)=O)nc21
CCOC(=O)c1cccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)c1
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
4829c7fa353840c036de48b4c116a7d68d2d5d8395d0f64d6e8c63d9a9bd4025
f263fb011eaf2f85af25e2af9b0908fb2797226f3495a5d6be9230bf229d4fae
O=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1ccccc1
C-S(=O)(=O)-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c:5](:[#7;a:6]:1):[#7;a:7](-[C;D1;H3:8]):[c:9].[NH2;D1;+0:10]-[c:11](:[c:12]):[c:13]>>[C;D1;H3:8]-[#7;a:7](:[c:9]):[c:5]1:[#7;a:6]:[c;H0;D3;+0:1](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[#7;a:2]:[c:3]:[c:4]:1
null
[]
100
CELSIUS
6
MINUTE
A mixture of 0.226 g (0.58 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.40 g (2.42 mmol) of 3-aminobenzoic acid, ethyl ester was fused in a 170° C. oil bath to give a clear melt. After 6 minutes, the melt was cooled to ca. 100° C. Glacial acetic acid (1 ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfone
Secondary amine
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1ccccc1.c1cnc2ncncc2c1.c1ccccc1
HO-
O
100
0.1
CCOC(=O)c1cccc(N)c1.Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(S(C)(=O)=O)nc21>O>CCOC(=O)c1cccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1b1496d4ad5040759352f2bc285c5252
CCOC(=O)c1cccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)c1>>Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3cccc(C(=O)O)c3)nc21
ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC=2C=C(C(=O)OCC)C=CC2)N(C1=O)C.[OH-].[Na+].C(C)(=O)O>>ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC=2C=C(C(=O)O)C=CC2)N(C1=O)C
CC[O:27][C:25]([c:24]1[cH:23][cH:22][cH:21][c:20]([NH:19][c:18]2[n:17][cH:16][c:15]3[cH:14][c:5](-[c:6]4[c:7]([Cl:8])[cH:9][cH:10][cH:11][c:12]4[Cl:13])[c:3](=[O:4])[n:2]([CH3:1])[c:30]3[n:29]2)[cH:28]1)=[O:26]>>[CH3:1][n:2]1[c:3](=[O:4])[c:5](-[c:6]2[c:7]([Cl:8])[cH:9][cH:10][cH:11][c:12]2[Cl:13])[cH:14][c:15]2[cH:16]...
CCOC(=O)c1cccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)c1
Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3cccc(C(=O)O)c3)nc21
null
null
CO
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1ccccc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4]>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4]
null
[]
null
null
null
null
A quantity of 0.065 g (0.139 mmol) of 3-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino]-benzoic acid, ethyl ester of Example 89 was dissolved in 75 mL of boiling methanol. 2N Sodium hydroxide (2 mL) was added, and the clear solution was maintained at reflux for 2 hours. The solution...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1cnc2ncncc2c1.c1ccccc1
Other
CO
null
null
CCOC(=O)c1cccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)c1>CO>Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3cccc(C(=O)O)c3)nc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a983572781e049c5930f6eb5910fc562
CCOC(=O)CCCc1ccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)cc1>>Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3ccc(CCCC(=O)O)cc3)nc21
[OH-].[Na+].ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC2=CC=C(C=C2)CCCC(=O)OCC)N(C1=O)C>>ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC2=CC=C(C=C2)CCCC(=O)O)N(C1=O)C
CC[O:29][C:27]([CH2:26][CH2:25][CH2:24][c:23]1[cH:22][cH:21][c:20]([NH:19][c:18]2[n:17][cH:16][c:15]3[cH:14][c:5](-[c:6]4[c:7]([Cl:8])[cH:9][cH:10][cH:11][c:12]4[Cl:13])[c:3](=[O:4])[n:2]([CH3:1])[c:33]3[n:32]2)[cH:31][cH:30]1)=[O:28]>>[CH3:1][n:2]1[c:3](=[O:4])[c:5](-[c:6]2[c:7]([Cl:8])[cH:9][cH:10][cH:11][c:12]2[Cl:1...
CCOC(=O)CCCc1ccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)cc1
Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3ccc(CCCC(=O)O)cc3)nc21
null
null
C(C)(=O)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1ccccc1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
34.5
[{"value": 34.5, "product": "ClC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC2=CC=C(C=C2)CCCC(=O)O)N(C1=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A volume of 5 mL of 2N sodium hydroxide was added to a hot stirred solution of 0.170 g (0.33 mmol) of 4-[4-{6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino]-phenyl}-butyric acid, ethyl ester of Example 91. The solution was maintained at reflux for 1 hour. Glacial acetic acid (1 mL) wa...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1cnc2ncncc2c1.c1ccccc1
Other
C(C)(=O)O
null
null
CCOC(=O)CCCc1ccc(Nc2ncc3cc(-c4c(Cl)cccc4Cl)c(=O)n(C)c3n2)cc1>C(C)(=O)O>Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(Nc3ccc(CCCC(=O)O)cc3)nc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-40e5a488e6884a15aae82381ce1c1729
CCN.CCOC(=O)c1cnc(SC)nc1Cl>>CCNc1nc(SC)ncc1C(=O)OCC
C(C)N.C(C)OC(=O)C=1C(=NC(=NC1)SC)Cl.C(C)N(CC)CC>>C(C)OC(=O)C=1C(=NC(=NC1)SC)NCC
[CH3:1][CH2:2][NH2:3].Cl[c:4]1[n:5][c:6]([S:7][CH3:8])[n:9][cH:10][c:11]1[C:12](=[O:13])[O:14][CH2:15][CH3:16]>>[CH3:1][CH2:2][NH:3][c:4]1[n:5][c:6]([S:7][CH3:8])[n:9][cH:10][c:11]1[C:12](=[O:13])[O:14][CH2:15][CH3:16]
CCN.CCOC(=O)c1cnc(SC)nc1Cl
CCNc1nc(SC)ncc1C(=O)OCC
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
c38b7155556ff28144ae37859ff6668b20d59da60c705d26b158542b6d8385da
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1cncnc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5]:[c:6]:1-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10].[C;D1;H3:11]-[C:12]-[NH2;D1;+0:13]>>[C:10]-[#8:9]-[C:7](=[O;D1;H0:8])-[c:6]1:[c:5]:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:1-[NH;D2;+0:13]-[C:12]-[C;D1;H3:11]
90
[{"value": 90.0, "product": "C(C)OC(=O)C=1C(=NC(=NC1)SC)NCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.6, "product": "C(C)OC(=O)C=1C(=NC(=NC1)SC)NCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a room temperature solution of 4-chloro-2-methylthio-5-pyrimidinecarboxylate ethyl ester (10.00 g, 43.10 mmol) in 150 mL of tetrahydrofuran was added triethylamine (18.5 mL, 133 mmol) followed by 9 mL of a 70% aqueous solution of ethylamine. The solution was stirred for 30 minutes, then concentrated in vacuo and par...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1cncnc1
c1cncnc1
c1cncnc1
HCl
O1CCCC1
null
0.5
CCN.CCOC(=O)c1cnc(SC)nc1Cl>O1CCCC1>CCNc1nc(SC)ncc1C(=O)OCC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f2375584c8354f2a9aff7eb95f5d470f
CCNc1nc(SC)ncc1C(=O)OCC>>CCNc1nc(SC)ncc1CO
C(C)OC(=O)C=1C(=NC(=NC1)SC)NCC.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>C(C)NC1=NC(=NC=C1CO)SC
CCO[C:12]([c:11]1[c:4]([NH:3][CH2:2][CH3:1])[n:5][c:6]([S:7][CH3:8])[n:9][cH:10]1)=[O:13]>>[CH3:1][CH2:2][NH:3][c:4]1[n:5][c:6]([S:7][CH3:8])[n:9][cH:10][c:11]1[CH2:12][OH:13]
CCNc1nc(SC)ncc1C(=O)OCC
CCNc1nc(SC)ncc1CO
null
null
O1CCCC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1cncnc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3]1:[c:4]:[#7;a:5]:[c:6]:[#7;a:7]:[c:8]:1-[#7:9]>>[#7:9]-[c:8]1:[#7;a:7]:[c:6]:[#7;a:5]:[c:4]:[c:3]:1-[CH2;D2;+0:1]-[OH;D1;+0:2]
92
[{"value": 92.0, "product": "C(C)NC1=NC(=NC=C1CO)SC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.6, "product": "C(C)NC1=NC(=NC=C1CO)SC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
A solution of 4-ethylamino-2-methylthio-5-pyrimidinecarboxylate ethyl ester (8.93 g, 37.1 mmol) in 100 mL of tetrahydrofuran was added dropwise to a room temperature suspension of lithium aluminum hydride (2.30 g, 60.5 mmol) in 100 mL of tetrahydrofuran. After 10 minutes, the reaction was carefully quenched with 4.5 mL...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1cncnc1
HO-
O1CCCC1
null
0.166667
CCNc1nc(SC)ncc1C(=O)OCC>O1CCCC1>CCNc1nc(SC)ncc1CO
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0f80dab124bd4936956f14f0363292fa
CCNc1nc(SC)ncc1CO>>CCNc1nc(SC)ncc1C=O
C(C)NC1=NC(=NC=C1CO)SC>>C(C)NC1=NC(=NC=C1C=O)SC
[CH3:1][CH2:2][NH:3][c:4]1[n:5][c:6]([S:7][CH3:8])[n:9][cH:10][c:11]1[CH2:12][OH:13]>>[CH3:1][CH2:2][NH:3][c:4]1[n:5][c:6]([S:7][CH3:8])[n:9][cH:10][c:11]1[CH:12]=[O:13]
CCNc1nc(SC)ncc1CO
CCNc1nc(SC)ncc1C=O
null
[O-2].[Mn+2].[O-2].[Mn+2]
C(Cl)(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1cncnc1
[#7:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1-[CH2;D2;+0:8]-[OH;D1;+0:9]>>[#7:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1-[CH;D2;+0:8]=[O;H0;D1;+0:9]
97.8
[{"value": 97.0, "product": "C(C)NC1=NC(=NC=C1C=O)SC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.8, "product": "C(C)NC1=NC(=NC=C1C=O)SC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To 4-ethylamino-2-methylthio-5-pyrimidinemethanol (6.44 g, 32.4 mmol) in 600 mL of chloroform was added manganese oxide (21.0 g, 241 mmol) over 3 minutes. The suspension was stirred at room temperature for 2 hours, and an additional 5.5 g of manganese oxide was added. Stirring was continued for 4.5 hours. The mixture w...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1cncnc1
null
[O-2].[Mn+2].[O-2].[Mn+2].C(Cl)(Cl)Cl
null
2
CCNc1nc(SC)ncc1CO>[O-2].[Mn+2].[O-2].[Mn+2].C(Cl)(Cl)Cl>CCNc1nc(SC)ncc1C=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d3784f90e3f54ca8a6dd0f00da8e8fa4
CCNc1nc(Nc2ccccc2)ncc1C(=O)OCC>>CCNc1nc(Nc2ccccc2)ncc1CO
C(C)OC(=O)C=1C(=NC(=NC1)NC1=CC=CC=C1)NCC.[H-].[Al+3].[Li+].[H-].[H-].[H-].[H-].[Al+3].[Li+].[H-].[H-].[H-]>>C(C)NC1=NC(=NC=C1CO)NC1=CC=CC=C1
CCO[C:17]([c:16]1[c:4]([NH:3][CH2:2][CH3:1])[n:5][c:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[n:14][cH:15]1)=[O:18]>>[CH3:1][CH2:2][NH:3][c:4]1[n:5][c:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[n:14][cH:15][c:16]1[CH2:17][OH:18]
CCNc1nc(Nc2ccccc2)ncc1C(=O)OCC
CCNc1nc(Nc2ccccc2)ncc1CO
null
null
O1CCCC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(Nc2ncccn2)cc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3]1:[c:4]:[#7;a:5]:[c:6]:[#7;a:7]:[c:8]:1-[#7:9]>>[#7:9]-[c:8]1:[#7;a:7]:[c:6]:[#7;a:5]:[c:4]:[c:3]:1-[CH2;D2;+0:1]-[OH;D1;+0:2]
39
[{"value": 39.0, "product": "C(C)NC1=NC(=NC=C1CO)NC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 38.8, "product": "C(C)NC1=NC(=NC=C1CO)NC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
25
MINUTE
A solution of 4-ethylamino-2-phenylamino-pyrimidine-5-carboxylic acid ethyl ester (109 mg, 0.38 mmol) in 6 mL of tetrahydrofuran was added dropwise to a room temperature suspension of lithium aluminum hydride (35 mg, 0.92 mmol) in 5 mL of tetrahydrofuran. After 25 minutes, an additional 30 mg of lithium aluminum hydrid...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1cncnc1.c1ccccc1
HO-
O1CCCC1
null
0.416667
CCNc1nc(Nc2ccccc2)ncc1C(=O)OCC>O1CCCC1>CCNc1nc(Nc2ccccc2)ncc1CO
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-01090b6109b34cf4ad06377fa270ba3b
CCNc1nc(Nc2ccccc2)ncc1CO>>CCNc1nc(Nc2ccccc2)ncc1C=O
C(C)NC1=NC(=NC=C1CO)NC1=CC=CC=C1>>C(C)NC1=NC(=NC=C1C=O)NC1=CC=CC=C1
[CH3:1][CH2:2][NH:3][c:4]1[n:5][c:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[n:14][cH:15][c:16]1[CH2:17][OH:18]>>[CH3:1][CH2:2][NH:3][c:4]1[n:5][c:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[n:14][cH:15][c:16]1[CH:17]=[O:18]
CCNc1nc(Nc2ccccc2)ncc1CO
CCNc1nc(Nc2ccccc2)ncc1C=O
null
[O-2].[Mn+2]
C(Cl)(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccc(Nc2ncccn2)cc1
[#7:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1-[CH2;D2;+0:8]-[OH;D1;+0:9]>>[#7:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1-[CH;D2;+0:8]=[O;H0;D1;+0:9]
99
[{"value": 99.0, "product": "C(C)NC1=NC(=NC=C1C=O)NC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.8, "product": "C(C)NC1=NC(=NC=C1C=O)NC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of (4-ethylamino-2-phenylamino-pyrimidin-5-yl)methanol (173 mg, 0.71 mmol) in 15 mL of chloroform was added manganese oxide (600 mg, 6.89 mmol). After stirring at room temperature overnight, the mixture was filtered through a pad of Celite, washing with chloroform. The filtrate was concentrated in vacuo t...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1cncnc1.c1ccccc1
null
[O-2].[Mn+2].C(Cl)(Cl)Cl
null
8
CCNc1nc(Nc2ccccc2)ncc1CO>[O-2].[Mn+2].C(Cl)(Cl)Cl>CCNc1nc(Nc2ccccc2)ncc1C=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5ac9e9c1c2b44b098f10a1ddc3f11428
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1ccsc1>>CCn1c(=N)c(-c2ccsc2)cc2cnc(Nc3ccccc3)nc21
O.S1C=C(C=C1)CC#N.[H-].[Na+].C(C)NC1=NC(=NC=C1C=O)NC1=CC=CC=C1>>C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C2=CSC=C2)=N
O=[CH:12][c:13]1[cH:14][n:15][c:16]([NH:17][c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)[n:24][c:25]1[NH:3][CH2:2][CH3:1].[C:4](#[N:5])[CH2:6][c:7]1[cH:8][cH:9][s:10][cH:11]1>>[CH3:1][CH2:2][n:3]1[c:4](=[NH:5])[c:6](-[c:7]2[cH:8][cH:9][s:10][cH:11]2)[cH:12][c:13]2[cH:14][n:15][c:16]([NH:17][c:18]3[cH:19][cH:20][cH:21][c...
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1ccsc1
CCn1c(=N)c(-c2ccsc2)cc2cnc(Nc3ccccc3)nc21
null
null
C(C)OCCO
Aromatic Heterocycle Formation
OtherReaction
0563001d31884c03e15e9f4307d31ffde7ef37fabfd8267db28237eb39076249
869483589005a5aba7d1617b2e2f826aa2ded09152e8d61d0607fd18c3c9c8b9
N=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1ccsc1
O=[CH;D2;+0:1]-[c:2]1:[c:3]:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:1-[NH;D2;+0:8]-[C:9]-[C;D1;H3:10].[N;H0;D1;+0:11]#[C;H0;D2;+0:12]-[CH2;D2;+0:13]-[c;H0;D3;+0:14]1:[c:15]:[#16;a:16]:[c:17]:[c:18]:1>>[C;D1;H3:10]-[C:9]-[n;H0;D3;+0:8]1:[c:7]2:[#7;a:6]:[c:5]:[#7;a:4]:[c:3]:[c:2]:2:[cH;D2;+0:1]:[c;H0;D3;+0:13](-[c;H0;D3;+0:14]2:[c...
78.9
[{"value": 78.0, "product": "C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C2=CSC=C2)=N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.9, "product": "C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C2=CSC=C2)=N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
To a suspension of NaH (60% in mineral oil, 27 mg) in 5 mL of 2-ethoxyethanol was added 3-thiopheneacetonitrile (168 mg, 1.36 mmol). After stirring for 5 minutes at room temperature, 4-ethylamino-2-phenylamino-pyrimidine-5-carbaldehyde (300 mg, 1.24 mmol) was added, and the reaction heated at 120° C. for 2 hours, resul...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Nitrile.Secondary amine
null
c1cncnc1
c1cnc2ncncc2c1
c1ccsc1.c1cnc2ncncc2c1.c1ccccc1
HO-
C(C)OCCO
null
0.083333
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1ccsc1>C(C)OCCO>CCn1c(=N)c(-c2ccsc2)cc2cnc(Nc3ccccc3)nc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-231cd6e88b2340b49783a8530c5952cf
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1cccs1>>CCn1c(=N)c(-c2cccs2)cc2cnc(Nc3ccccc3)nc21
O.S1C(=CC=C1)CC#N.[H-].[Na+].C(C)NC1=NC(=NC=C1C=O)NC1=CC=CC=C1>>C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C=2SC=CC2)=N
O=[CH:12][c:13]1[cH:14][n:15][c:16]([NH:17][c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)[n:24][c:25]1[NH:3][CH2:2][CH3:1].[C:4](#[N:5])[CH2:6][c:7]1[cH:8][cH:9][cH:10][s:11]1>>[CH3:1][CH2:2][n:3]1[c:4](=[NH:5])[c:6](-[c:7]2[cH:8][cH:9][cH:10][s:11]2)[cH:12][c:13]2[cH:14][n:15][c:16]([NH:17][c:18]3[cH:19][cH:20][cH:21][c...
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1cccs1
CCn1c(=N)c(-c2cccs2)cc2cnc(Nc3ccccc3)nc21
null
null
C(C)OCCO
Aromatic Heterocycle Formation
OtherReaction
0563001d31884c03e15e9f4307d31ffde7ef37fabfd8267db28237eb39076249
869483589005a5aba7d1617b2e2f826aa2ded09152e8d61d0607fd18c3c9c8b9
N=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1cccs1
O=[CH;D2;+0:1]-[c:2]1:[c:3]:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:1-[NH;D2;+0:8]-[C:9]-[C;D1;H3:10].[N;H0;D1;+0:11]#[C;H0;D2;+0:12]-[CH2;D2;+0:13]-[c;H0;D3;+0:14]1:[#16;a:15]:[c:16]:[c:17]:[c:18]:1>>[C;D1;H3:10]-[C:9]-[n;H0;D3;+0:8]1:[c:7]2:[#7;a:6]:[c:5]:[#7;a:4]:[c:3]:[c:2]:2:[cH;D2;+0:1]:[c;H0;D3;+0:13](-[c;H0;D3;+0:14]2:[#...
85.9
[{"value": 85.0, "product": "C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C=2SC=CC2)=N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 85.9, "product": "C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C=2SC=CC2)=N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
To a suspension of NaH (60% in mineral oil, 27 mg) in 5 mL of 2-ethoxyethanol was added 2-thiopheneacetonitrile (168 mg, 1.36 mmol). After stirring for 5 minutes at room temperature, 4-ethylamino-2-phenylamino-pyrimidine-5-carbaldehyde (300 mg, 1.24 mmol) was added, and the reaction heated at 120° C. for 2 hours, resul...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Nitrile.Secondary amine
null
c1cncnc1
c1cnc2ncncc2c1
c1ccsc1.c1cnc2ncncc2c1.c1ccccc1
HO-
C(C)OCCO
null
0.083333
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1cccs1>C(C)OCCO>CCn1c(=N)c(-c2cccs2)cc2cnc(Nc3ccccc3)nc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8101dbefc33b4ad5952d74a7f2f862b6
CC(=O)OC(C)=O.CCn1c(=N)c(-c2c(Cl)cccc2Br)cc2cnc(Nc3ccccc3)nc21>>CCn1c(=O)c(-c2c(Cl)cccc2Br)cc2cnc(Nc3ccccc3)nc21
BrC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC2=CC=CC=C2)N(C1=N)CC.C(C)(=O)OC(C)=O.Cl>>BrC1=C(C(=CC=C1)Cl)C1=CC2=C(N=C(N=C2)NC2=CC=CC=C2)N(C1=O)CC
CC(=O)OC(C)=[O:5].N=[c:4]1[n:3]([CH2:2][CH3:1])[c:28]2[c:16]([cH:15][c:6]1-[c:7]1[c:8]([Cl:9])[cH:10][cH:11][cH:12][c:13]1[Br:14])[cH:17][n:18][c:19]([NH:20][c:21]1[cH:22][cH:23][cH:24][cH:25][cH:26]1)[n:27]2>>[CH3:1][CH2:2][n:3]1[c:4](=[O:5])[c:6](-[c:7]2[c:8]([Cl:9])[cH:10][cH:11][cH:12][c:13]2[Br:14])[cH:15][c:16]2[...
CC(=O)OC(C)=O.CCn1c(=N)c(-c2c(Cl)cccc2Br)cc2cnc(Nc3ccccc3)nc21
CCn1c(=O)c(-c2c(Cl)cccc2Br)cc2cnc(Nc3ccccc3)nc21
null
null
O
Miscellaneous
OtherReaction
dd6199f82f5f25315dda3b0cdb80b809165964de59b82b4515ab2b9ff97290b0
41e7ec317aa33bd872bc25f64db351112544c3e9bc552c10a46e7a1666c9e76a
O=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1ccccc1
C-C(=O)-O-C(-C)=[O;H0;D1;+0:1].N=[c;H0;D3;+0:2](:[#7;a:3](-[C:4]):[c:5]:[#7;a:6]):[c:7](-[c:8]):[c:9]>>[#7;a:6]:[c:5]:[#7;a:3](-[C:4]):[c;H0;D3;+0:2](=[O;H0;D1;+0:1]):[c:7](-[c:8]):[c:9]
null
[]
null
null
null
null
(6-(2-Bromo-6-chlorophenyl)-8-ethyl-7-imino-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl)-phenylamine (150 mg) was added to 1 mL of acetic anhydride and heated at reflux for 5 minutes. The reaction was cooled and concentrated resulting in an oil which was heated at reflux with 10 mL of 6N HCl for 10 minutes. The reaction wa...
10.6084/m9.figshare.5104873.v1
null
Anhydride
null
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1ccccc1.c1cnc2ncncc2c1.c1ccccc1
HO-
O
null
null
CC(=O)OC(C)=O.CCn1c(=N)c(-c2c(Cl)cccc2Br)cc2cnc(Nc3ccccc3)nc21>O>CCn1c(=O)c(-c2c(Cl)cccc2Br)cc2cnc(Nc3ccccc3)nc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-abec610d41fa4460bcec11b0f48f849d
CC(C)(C)OC(=O)Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(N)nc21>>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(CC(=O)O)c2n1
C(C)OCC.C(C)(C)(C)OC(CN1C(C(=CC2=C1N=C(N=C2)N)C2=C(C=CC=C2Cl)Cl)=O)=O.FC(C(=O)O)(F)F>>NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC(=O)O
CC(C)(C)[O:22][C:20]([CH2:19][n:18]1[c:16](=[O:17])[c:7](-[c:8]2[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]2[Cl:15])[cH:6][c:5]2[cH:4][n:3][c:2]([NH2:1])[n:24][c:23]21)=[O:21]>>[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17])[n:18]([CH2:19][C:20](=[O:21])[...
CC(C)(C)OC(=O)Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(N)nc21
Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(CC(=O)O)c2n1
null
null
C(Cl)Cl
Deprotection
Deprotection of carboxylic acid
152e5537e48c95b4a3e767536b0f9f68d1308e5f484070828ab5ed951805157a
7f019d4cfe9b3036d0a2d3a3209aa0e1fcb05418ebee15a4be5e125d315d5f01
O=c1[nH]c2ncncc2cc1-c1ccccc1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
52.5
[{"value": 52.0, "product": "NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC(=O)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 52.5, "product": "NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
To a solution of [2-amino-6-(2,6-dichlorophenyl)-7-oxo-7H-pyrido[2,3-d]pyrimidin-8-yl]-acetic acid tert-butyl ester (157 mg, 0.37 mmol) from Example 36 in 4 mL of methylene chloride was added 2 mL of trifluoroacetic acid. The solution was stirred at room temperature for 5 hours, then concentrated in vacuo. The resultan...
10.6084/m9.figshare.5104873.v1
null
Ester.Boc
Carboxylic acid
null
null
c1cnc2ncncc2c1.c1ccccc1
Other
C(Cl)Cl
null
5
CC(C)(C)OC(=O)Cn1c(=O)c(-c2c(Cl)cccc2Cl)cc2cnc(N)nc21>C(Cl)Cl>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(CC(=O)O)c2n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d37a984a916b40a38246819bac9f0f12
BrCc1cccc(Br)c1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3cccc(Br)c3)c2n1
NC=1N=CC2=C(N1)NC(C(=C2)C2=C(C=CC=C2Cl)Cl)=O.[H-].[Na+].BrC=1C=C(CBr)C=CC1>>NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC2=CC(=CC=C2)Br
Br[CH2:19][c:20]1[cH:21][cH:22][cH:23][c:24]([Br:25])[cH:26]1.[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17])[nH:18][c:27]2[n:28]1>>[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17])[n:18](...
BrCc1cccc(Br)c1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1
Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3cccc(Br)c3)c2n1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
c0bd97f4a1ce12437e73bb376c2b79161100c8750c084a20105c044989ac3551
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=c1c(-c2ccccc2)cc2cncnc2n1Cc1ccccc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[c:6](:[c:7]):[nH;D2;+0:8]:[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1>>[O;D1;H0:5]=[c:6](:[c:7]):[n;H0;D3;+0:8](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]):[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1
58
[{"value": 58.0, "product": "NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC2=CC(=CC=C2)Br", "details": "PERCENTYIELD", "is_desired": false}, {"value": 57.5, "product": "NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC2=CC(=CC=C2)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
10
MINUTE
To a suspension of NaH (60% in mineral oil, 38 mg) in 8 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (200 mg, 0.65 mmol). The mixture was heated at 50° C. for 20 minutes resulting in a clear solution. The heating mantle was removed, and 3-bromobenzyl bromide (240 μL,...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1cnc2ncncc2c1.c1ccccc1.c1ccccc1
HBr
CN(C=O)C
50
0.166667
BrCc1cccc(Br)c1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>CN(C=O)C>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3cccc(Br)c3)c2n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-145f75e858214880a64bbd4992e3190e
COC(=O)c1ccc(CBr)cc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>>COC(=O)c1ccc(Cn2c(=O)c(-c3c(Cl)cccc3Cl)cc3cnc(N)nc32)cc1
[H-].[Na+].C(C)(=O)OCC.NC=1N=CC2=C(N1)NC(C(=C2)C2=C(C=CC=C2Cl)Cl)=O.COC(=O)C1=CC=C(C=C1)CBr>>COC(C1=CC=C(C=C1)CN1C(C(=CC2=C1N=C(N=C2)N)C2=C(C=CC=C2Cl)Cl)=O)=O
Br[CH2:9][c:8]1[cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:31][cH:30]1.[nH:10]1[c:11](=[O:12])[c:13](-[c:14]2[c:15]([Cl:16])[cH:17][cH:18][cH:19][c:20]2[Cl:21])[cH:22][c:23]2[cH:24][n:25][c:26]([NH2:27])[n:28][c:29]12>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH2:9][n:10]2[c:11](=[O:12])[c:13](-[c:14]3[c:1...
COC(=O)c1ccc(CBr)cc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1
COC(=O)c1ccc(Cn2c(=O)c(-c3c(Cl)cccc3Cl)cc3cnc(N)nc32)cc1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
c0bd97f4a1ce12437e73bb376c2b79161100c8750c084a20105c044989ac3551
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=c1c(-c2ccccc2)cc2cncnc2n1Cc1ccccc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[c:6](:[c:7]):[nH;D2;+0:8]:[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1>>[O;D1;H0:5]=[c:6](:[c:7]):[n;H0;D3;+0:8](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]):[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1
70
[{"value": 70.0, "product": "COC(C1=CC=C(C=C1)CN1C(C(=CC2=C1N=C(N=C2)N)C2=C(C=CC=C2Cl)Cl)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a suspension of NaH (60% in mineral oil, 36 mg) in 7 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (195 mg, 0.64 mmol). The mixture was heated at 40° C. to 50° C. for 20 minutes, resulting in a clear solution. Methyl 4-(bromomethyl) benzoate (206 mg, 0.90 mmol) was...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1ccccc1.c1ccccc1.c1cnc2ncncc2c1
HBr
CN(C=O)C
null
null
COC(=O)c1ccc(CBr)cc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>CN(C=O)C>COC(=O)c1ccc(Cn2c(=O)c(-c3c(Cl)cccc3Cl)cc3cnc(N)nc32)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-eccbafead2a446cdb38d33e16b8e1e3f
Clc1cccc(Cl)c1CBr.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3c(Cl)cccc3Cl)c2n1
[H-].[Na+].NC=1N=CC2=C(N1)NC(C(=C2)C2=C(C=CC=C2Cl)Cl)=O.BrCC1=C(C=CC=C1Cl)Cl>>NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC2=C(C=CC=C2Cl)Cl
Br[CH2:19][c:20]1[c:21]([Cl:22])[cH:23][cH:24][cH:25][c:26]1[Cl:27].[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17])[nH:18][c:28]2[n:29]1>>[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17])[...
Clc1cccc(Cl)c1CBr.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1
Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3c(Cl)cccc3Cl)c2n1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
c0bd97f4a1ce12437e73bb376c2b79161100c8750c084a20105c044989ac3551
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=c1c(-c2ccccc2)cc2cncnc2n1Cc1ccccc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[c:6](:[c:7]):[nH;D2;+0:8]:[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1>>[O;D1;H0:5]=[c:6](:[c:7]):[n;H0;D3;+0:8](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]):[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1
35.3
[{"value": 35.0, "product": "NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC2=C(C=CC=C2Cl)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 35.3, "product": "NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC2=C(C=CC=C2Cl)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
30
MINUTE
To a suspension of NaH (60% in mineral oil, 36 mg) in 8 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (208 mg, 0.68 mmol). The mixture was heated at 70° C. for 10 minutes and then at 50° C. for 30 minutes, resulting in a clear solution. α-Bromo-2,6-dichlorotoluene (21...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1cnc2ncncc2c1.c1ccccc1.c1ccccc1
HBr
CN(C=O)C
70
0.5
Clc1cccc(Cl)c1CBr.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>CN(C=O)C>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3c(Cl)cccc3Cl)c2n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-afbdbf0f072e4583b666e79f728d3640
COc1ccc(CCl)cc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>>COc1ccc(Cn2c(=O)c(-c3c(Cl)cccc3Cl)cc3cnc(N)nc32)cc1
COC1=CC=C(CCl)C=C1.[H-].[Na+].NC=1N=CC2=C(N1)NC(C(=C2)C2=C(C=CC=C2Cl)Cl)=O>>NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC2=CC=C(C=C2)OC
Cl[CH2:7][c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:29][cH:28]1.[nH:8]1[c:9](=[O:10])[c:11](-[c:12]2[c:13]([Cl:14])[cH:15][cH:16][cH:17][c:18]2[Cl:19])[cH:20][c:21]2[cH:22][n:23][c:24]([NH2:25])[n:26][c:27]12>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][n:8]2[c:9](=[O:10])[c:11](-[c:12]3[c:13]([Cl:14])[cH:15][cH:16][cH:1...
COc1ccc(CCl)cc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1
COc1ccc(Cn2c(=O)c(-c3c(Cl)cccc3Cl)cc3cnc(N)nc32)cc1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
c0bd97f4a1ce12437e73bb376c2b79161100c8750c084a20105c044989ac3551
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=c1c(-c2ccccc2)cc2cncnc2n1Cc1ccccc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[c:6](:[c:7]):[nH;D2;+0:8]:[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1>>[O;D1;H0:5]=[c:6](:[c:7]):[n;H0;D3;+0:8](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]):[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1
72
[{"value": 72.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
50
CELSIUS
null
null
To a suspension of NaH (60% in mineral oil, 38 mg) in 8 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (208 mg, 0.68 mmol). The mixture was heated at 50° C. for 1 hour, resulting in a clear solution. 4-Methoxybenzyl chloride (130 μL, 0.95 mmol) was added, and the react...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1ccccc1.c1ccccc1.c1cnc2ncncc2c1
HCl
CN(C=O)C
50
null
COc1ccc(CCl)cc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>CN(C=O)C>COc1ccc(Cn2c(=O)c(-c3c(Cl)cccc3Cl)cc3cnc(N)nc32)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d68719fd07424782a508df3f799b02af
ClCc1ccncc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3ccncc3)c2n1
Cl.N1=CC=C(C=C1)CCl.[Na].NC=1N=CC2=C(N1)NC(C(=C2)C2=C(C=CC=C2Cl)Cl)=O.NC=1N=CC2=C(N1)NC(C(=C2)C2=C(C=CC=C2Cl)Cl)=O.C(C)N(CC)CC.[H-].[Na+]>>NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CC2=CC=NC=C2
Cl[CH2:19][c:20]1[cH:21][cH:22][n:23][cH:24][cH:25]1.[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17])[nH:18][c:26]2[n:27]1>>[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17])[n:18]([CH2:19][...
ClCc1ccncc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1
Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3ccncc3)c2n1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
c0bd97f4a1ce12437e73bb376c2b79161100c8750c084a20105c044989ac3551
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=c1c(-c2ccccc2)cc2cncnc2n1Cc1ccncc1
Cl-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1.[O;D1;H0:8]=[c:9](:[c:10]):[nH;D2;+0:11]:[c:12]1:[#7;a:13]:[c:14]:[#7;a:15]:[c:16]:[c:17]:1>>[O;D1;H0:8]=[c:9](:[c:10]):[n;H0;D3;+0:11](-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1):[c:12]1:[#7;a:13]:[c:14]:[#7;a:15]:[c:16]:[c:17]:1
null
[]
70
CELSIUS
null
null
To a suspension of NaH (60% in mineral oil, 32 mg) in 6 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (200 mg, 0.65 mmol) and the mixture heated to 70° C. In a second flask containing triethyl amine (220 μL, 1.59 mmol) in 4 mL of dimethylformamide was added 4-picolyl ...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1cnc2ncncc2c1.c1ccccc1.c1ccncc1
HCl
CN(C=O)C
70
null
ClCc1ccncc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>CN(C=O)C>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(Cc3ccncc3)c2n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ce2698e35bd94905bfdf55ec0d5c3c0a
ClCCCc1ccccc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(CCCc3ccccc3)c2n1
[H-].[Na+].NC=1N=CC2=C(N1)NC(C(=C2)C2=C(C=CC=C2Cl)Cl)=O.ClCCCC1=CC=CC=C1>>NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CCCC2=CC=CC=C2
Cl[CH2:19][CH2:20][CH2:21][c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1.[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17])[nH:18][c:28]2[n:29]1>>[NH2:1][c:2]1[n:3][cH:4][c:5]2[cH:6][c:7](-[c:8]3[c:9]([Cl:10])[cH:11][cH:12][cH:13][c:14]3[Cl:15])[c:16](=[O:17]...
ClCCCc1ccccc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1
Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(CCCc3ccccc3)c2n1
null
null
CN(C=O)C.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
c0bd97f4a1ce12437e73bb376c2b79161100c8750c084a20105c044989ac3551
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=c1c(-c2ccccc2)cc2cncnc2n1CCCc1ccccc1
Cl-[CH2;D2;+0:1]-[C:2]-[C:3].[O;D1;H0:4]=[c:5](:[c:6]):[nH;D2;+0:7]:[c:8]1:[#7;a:9]:[c:10]:[#7;a:11]:[c:12]:[c:13]:1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:7](:[c:5](=[O;D1;H0:4]):[c:6]):[c:8]1:[#7;a:9]:[c:10]:[#7;a:11]:[c:12]:[c:13]:1
57.2
[{"value": 57.0, "product": "NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CCCC2=CC=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 57.2, "product": "NC=1N=CC2=C(N1)N(C(C(=C2)C2=C(C=CC=C2Cl)Cl)=O)CCCC2=CC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
null
null
To a suspension of NaH (60% in mineral oil, 58 mg) in 10 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (320 mg, 1.04 mmol). The mixture was heated to 60° C. resulting in a clear solution. 1-Chloro-3-phenylpropane (260 μL, 1.81 mmol) was added, and the reaction mixture...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1cnc2ncncc2c1.c1ccccc1.c1ccccc1
HCl
CN(C=O)C.C(C)(=O)OCC
60
null
ClCCCc1ccccc1.Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)[nH]c2n1>CN(C=O)C.C(C)(=O)OCC>Nc1ncc2cc(-c3c(Cl)cccc3Cl)c(=O)n(CCCc3ccccc3)c2n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5004f689fe8441b7b8fb304853ccbbc3
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1ccc2ccccc2c1>>CCn1c(=N)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21
O.C1=C(C=CC2=CC=CC=C12)CC#N.[H-].[Na+].C(C)NC1=NC(=NC=C1C=O)NC1=CC=CC=C1>>C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C2=CC1=CC=CC=C1C=C2)=N
O=[CH:17][c:18]1[cH:19][n:20][c:21]([NH:22][c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[n:29][c:30]1[NH:3][CH2:2][CH3:1].[C:4](#[N:5])[CH2:6][c:7]1[cH:8][cH:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[cH:16]1>>[CH3:1][CH2:2][n:3]1[c:4](=[NH:5])[c:6](-[c:7]2[cH:8][cH:9][c:10]3[cH:11][cH:12][cH:13][cH:14][c:15]3[cH:16]2...
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1ccc2ccccc2c1
CCn1c(=N)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21
null
null
C(C)OCCO
Aromatic Heterocycle Formation
OtherReaction
0563001d31884c03e15e9f4307d31ffde7ef37fabfd8267db28237eb39076249
869483589005a5aba7d1617b2e2f826aa2ded09152e8d61d0607fd18c3c9c8b9
N=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1ccc2ccccc2c1
O=[CH;D2;+0:1]-[c:2]1:[c:3]:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:1-[NH;D2;+0:8]-[C:9]-[C;D1;H3:10].[N;H0;D1;+0:11]#[C;H0;D2;+0:12]-[CH2;D2;+0:13]-[c;H0;D3;+0:14](:[c:15]:[c:16]):[c:17]:[c:18]>>[C;D1;H3:10]-[C:9]-[n;H0;D3;+0:8]1:[c:7]2:[#7;a:6]:[c:5]:[#7;a:4]:[c:3]:[c:2]:2:[cH;D2;+0:1]:[c;H0;D3;+0:13](-[c;H0;D3;+0:14](:[c:15]:...
82.4
[{"value": 82.0, "product": "C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C2=CC1=CC=CC=C1C=C2)=N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.4, "product": "C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C2=CC1=CC=CC=C1C=C2)=N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
To a suspension of NaH (60% in mineral oil, 27 mg) in 5 mL of 2-ethoxyethanol was added 2-naphthyl-acetonitrile (227 mg, 1.36 mmol). After stirring for 5 minutes at room temperature, 4-ethylamino-2-phenylamino-pyrimidine-5-carbaldehyde (300 mg, 1.24 mmol) was added and the reaction heated at 110° C. for 1 hour, resulti...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Nitrile.Secondary amine
null
c1cncnc1
c1cnc2ncncc2c1
c1ccc2ccccc2c1.c1cnc2ncncc2c1.c1ccccc1
HO-
C(C)OCCO
null
0.083333
CCNc1nc(Nc2ccccc2)ncc1C=O.N#CCc1ccc2ccccc2c1>C(C)OCCO>CCn1c(=N)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-bbffcf2db8554d41a139114578bcbcd5
CC(=O)OC(C)=O.CCn1c(=N)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21>>CCn1c(=O)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21
C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C2=CC1=CC=CC=C1C=C2)=N.C(C)(=O)OC(C)=O.Cl>>C(C)N1C(C(=CC2=C1N=C(N=C2)NC2=CC=CC=C2)C2=CC1=CC=CC=C1C=C2)=O
CC(=O)OC(C)=[O:5].N=[c:4]1[n:3]([CH2:2][CH3:1])[c:30]2[c:18]([cH:17][c:6]1-[c:7]1[cH:8][cH:9][c:10]3[cH:11][cH:12][cH:13][cH:14][c:15]3[cH:16]1)[cH:19][n:20][c:21]([NH:22][c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1)[n:29]2>>[CH3:1][CH2:2][n:3]1[c:4](=[O:5])[c:6](-[c:7]2[cH:8][cH:9][c:10]3[cH:11][cH:12][cH:13][cH:14][c:...
CC(=O)OC(C)=O.CCn1c(=N)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21
CCn1c(=O)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21
null
null
O
Miscellaneous
OtherReaction
dd6199f82f5f25315dda3b0cdb80b809165964de59b82b4515ab2b9ff97290b0
41e7ec317aa33bd872bc25f64db351112544c3e9bc552c10a46e7a1666c9e76a
O=c1[nH]c2nc(Nc3ccccc3)ncc2cc1-c1ccc2ccccc2c1
C-C(=O)-O-C(-C)=[O;H0;D1;+0:1].N=[c;H0;D3;+0:2](:[#7;a:3](-[C:4]):[c:5]:[#7;a:6]):[c:7](-[c:8]):[c:9]>>[#7;a:6]:[c:5]:[#7;a:3](-[C:4]):[c;H0;D3;+0:2](=[O;H0;D1;+0:1]):[c:7](-[c:8]):[c:9]
null
[]
null
null
null
null
(8-Ethyl-7-imino-6-naphthalen-2-yl-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl)-phenylamine (150 mg) was added to 1 mL of acetic anhydride and heated at reflux for 2 minutes. The reaction was cooled and concentrated, resulting in an oil which was heated at reflux with 10 mL of 6N HCl for 10 minutes. The reaction was cooled...
10.6084/m9.figshare.5104873.v1
null
Anhydride
null
c1cnc2ncncc2c1
c1cnc2ncncc2c1
c1ccc2ccccc2c1.c1cnc2ncncc2c1.c1ccccc1
HO-
O
null
null
CC(=O)OC(C)=O.CCn1c(=N)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21>O>CCn1c(=O)c(-c2ccc3ccccc3c2)cc2cnc(Nc3ccccc3)nc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ee329cf9c57341ee87f8398d0e4b9f66
ClCc1ccccn1.O=C1CNC(=S)N1>>O=C1CNC(SCc2ccccn2)=N1
N1C(=S)NC(=O)C1.C[O-].[Na+].Cl.ClCC1=NC=CC=C1>>N1=C(C=CC=C1)CSC=1NCC(N1)=O
Cl[CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][n:13]1.[O:1]=[C:2]1[CH2:3][NH:4][C:5](=[S:6])[NH:14]1>>[O:1]=[C:2]1[CH2:3][NH:4][C:5]([S:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]2)=[N:14]1
ClCc1ccccn1.O=C1CNC(=S)N1
O=C1CNC(SCc2ccccn2)=N1
null
null
CO
Protection
OtherReaction
46cef1e48600fcd6705529550ccb17b294e17c854f6cacd0473e52ed0910cca7
f72dba6c0cce6a796ff9aeda8637cc446706f96a34b889e05557c4a922c09746
O=C1CNC(SCc2ccccn2)=N1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[O;D1;H0:6]=[C:7]1-[C:8]-[#7:9]-[C;H0;D3;+0:10](=[S;H0;D1;+0:11])-[NH;D2;+0:12]-1>>[O;D1;H0:6]=[C:7]1-[C:8]-[#7:9]-[C;H0;D3;+0:10](-[S;H0;D2;+0:11]-[CH2;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5])=[N;H0;D2;+0:12]-1
null
[]
null
null
null
null
Initially, 1 g of 2-thiohydantoin and 2.5 g of sodium methylate were dissolved in 50 mL of methanol (MeoH), and 1.5 g of 2-chloromethylpyridine hydrochloride was added to the solution. The reaction mixture was stirred under reflux for one and a half hour and concentrated in vacuo. To the residue, there was added 50 mL ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea
Monosulfide
C1CNCN1
C1=NCCN1
C1=NCCN1.c1ccncc1
HCl
CO
null
null
ClCc1ccccn1.O=C1CNC(=S)N1>CO>O=C1CNC(SCc2ccccn2)=N1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f1dc421f62bb4c91b491d7738aa0887d
CC1(C)NC(=S)NC1=O.CN(C)c1ccccc1CCl>>CN(C)c1ccccc1CSC1=NC(=O)C(C)(C)N1
[OH-].[Na+].Cl.CN(C1=C(CCl)C=CC=C1)C.CC1(C(NC(N1)=S)=O)C.O>>CN(C1=C(CSC=2NC(C(N2)=O)(C)C)C=CC=C1)C
[S:11]=[C:12]1[NH:13][C:14](=[O:15])[C:16]([CH3:17])([CH3:18])[NH:19]1.Cl[CH2:10][c:9]1[c:4]([N:2]([CH3:1])[CH3:3])[cH:5][cH:6][cH:7][cH:8]1>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[CH2:10][S:11][C:12]1=[N:13][C:14](=[O:15])[C:16]([CH3:17])([CH3:18])[NH:19]1
CC1(C)NC(=S)NC1=O.CN(C)c1ccccc1CCl
CN(C)c1ccccc1CSC1=NC(=O)C(C)(C)N1
null
null
CS(=O)C
Protection
OtherReaction
46cef1e48600fcd6705529550ccb17b294e17c854f6cacd0473e52ed0910cca7
f72dba6c0cce6a796ff9aeda8637cc446706f96a34b889e05557c4a922c09746
O=C1CNC(SCc2ccccc2)=N1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C:6]1-[C:7]-[#7:8]-[C;H0;D3;+0:9](=[S;H0;D1;+0:10])-[NH;D2;+0:11]-1>>[O;D1;H0:5]=[C:6]1-[C:7]-[#7:8]-[C;H0;D3;+0:9](-[S;H0;D2;+0:10]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])=[N;H0;D2;+0:11]-1
null
[]
null
null
1
HOUR
Initially, 1 g of 5,5-dimethyl-2-thiohydantoin was dissolved in 20 mL of dimethylsulfoxide, and 1.7 g of 2-dimethylaminobenzylchloride hydrochloride was added to the solution. The reaction mixture was stirred at the room temperature for one hour, and poured into 50 mL of water. The pH value of the solution was adjusted...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea
Monosulfide
C1CNCN1
C1=NCCN1
c1ccccc1.C1=NCCN1
HCl
CS(=O)C
null
1
CC1(C)NC(=S)NC1=O.CN(C)c1ccccc1CCl>CS(=O)C>CN(C)c1ccccc1CSC1=NC(=O)C(C)(C)N1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e2a38ef21493407faefa7a6e38761e24
CC(=O)N1C(=S)NC(=O)C1(C)C.CN(C)c1ccccc1CCl>>CC(=O)N1C(SCc2ccccc2N(C)C)=NC(=O)C1(C)C
Cl.CN(C1=C(CCl)C=CC=C1)C.C(C)(=O)N1C(=S)NC(=O)C1(C)C.[OH-].[Na+]>>C(C)(=O)N1C(=NC(C1(C)C)=O)SCC1=C(C=CC=C1)N(C)C
[CH3:1][C:2](=[O:3])[N:4]1[C:5](=[S:6])[NH:17][C:18](=[O:19])[C:20]1([CH3:21])[CH3:22].Cl[CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][c:13]1[N:14]([CH3:15])[CH3:16]>>[CH3:1][C:2](=[O:3])[N:4]1[C:5]([S:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[N:14]([CH3:15])[CH3:16])=[N:17][C:18](=[O:19])[C:20]1([CH3:21])[CH3:22]
CC(=O)N1C(=S)NC(=O)C1(C)C.CN(C)c1ccccc1CCl
CC(=O)N1C(SCc2ccccc2N(C)C)=NC(=O)C1(C)C
null
null
O
Protection
OtherReaction
06d9f5797382049cde551f4363f7a6db1ae0ad2d934c141a8c10a407d5578211
f72dba6c0cce6a796ff9aeda8637cc446706f96a34b889e05557c4a922c09746
O=C1CNC(SCc2ccccc2)=N1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C;D1;H3:5]-[C:6](=[O;D1;H0:7])-[#7:8]1-[C:9]-[C:10](=[O;D1;H0:11])-[NH;D2;+0:12]-[C;H0;D3;+0:13]-1=[S;H0;D1;+0:14]>>[C;D1;H3:5]-[C:6](=[O;D1;H0:7])-[#7:8]1-[C:9]-[C:10](=[O;D1;H0:11])-[N;H0;D2;+0:12]=[C;H0;D3;+0:13]-1-[S;H0;D2;+0:14]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
1
HOUR
Initially, 4.18g of 2-dimethylaminobenzylchloride hydrochloride was added to a solution of 3.43 g of 1-N-acetyl-5,5-dimethyl-2-thiohydantoin in 50 mL of N,N-dimethylsulfoxide. The reaction mixture was stirred for one hour at the room temperature and poured into 100 mL of water. The pH of the solution was adjusted to 7-...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea
Monosulfide
C1C[NH]CN1
C1=NCC[NH]1
C1=NCC[NH]1.c1ccccc1
HCl
O
null
1
CC(=O)N1C(=S)NC(=O)C1(C)C.CN(C)c1ccccc1CCl>O>CC(=O)N1C(SCc2ccccc2N(C)C)=NC(=O)C1(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e6678ac22aa94fabbc9a581571db8c5e
CCC1(C)C(=O)NC(=S)N1C(C)=O.CN(C)c1ccccc1CCl>>CCC1(C)C(=O)N=C(SCc2ccccc2N(C)C)N1C(C)=O
Cl.CN(C1=C(CCl)C=CC=C1)C.C(C)(=O)N1C(=S)NC(=O)C1(C)CC>>C(C)(=O)N1C(=NC(C1(C)CC)=O)SCC1=C(C=CC=C1)N(C)C
[CH3:1][CH2:2][C:3]1([CH3:4])[C:5](=[O:6])[NH:7][C:8](=[S:9])[N:20]1[C:21]([CH3:22])=[O:23].Cl[CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][c:16]1[N:17]([CH3:18])[CH3:19]>>[CH3:1][CH2:2][C:3]1([CH3:4])[C:5](=[O:6])[N:7]=[C:8]([S:9][CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[N:17]([CH3:18])[CH3:19])[N:20]1[C:21]([C...
CCC1(C)C(=O)NC(=S)N1C(C)=O.CN(C)c1ccccc1CCl
CCC1(C)C(=O)N=C(SCc2ccccc2N(C)C)N1C(C)=O
null
null
null
Protection
OtherReaction
c436e84a346efd362c8a87a765b28845692c52ac6abb03e951ff1b63a6e85de9
f72dba6c0cce6a796ff9aeda8637cc446706f96a34b889e05557c4a922c09746
O=C1CNC(SCc2ccccc2)=N1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C;D1;H3:5]-[C:6](=[O;D1;H0:7])-[#7:8]1-[C:9]-[C:10](=[O;D1;H0:11])-[NH;D2;+0:12]-[C;H0;D3;+0:13]-1=[S;H0;D1;+0:14]>>[C;D1;H3:5]-[C:6](=[O;D1;H0:7])-[#7:8]1-[C:9]-[C:10](=[O;D1;H0:11])-[N;H0;D2;+0:12]=[C;H0;D3;+0:13]-1-[S;H0;D2;+0:14]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
In the present Example, 2.27 g of 2-dimethylaminobenzylchloride hydrochloride and 2.0 g of 1-N-acetyl-5-ethyl-5-methyl-2-thiohydantoin were reacted following the procedure of Example 33. The desired compound was obtained in the form of needle-like crystal. The yield of this compound was 1.37 g with a yield ratio of 41....
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea
Monosulfide
C1CNC[NH]1
C1=NCC[NH]1
C1=NCC[NH]1.c1ccccc1
HCl
null
null
null
CCC1(C)C(=O)NC(=S)N1C(C)=O.CN(C)c1ccccc1CCl>>CCC1(C)C(=O)N=C(SCc2ccccc2N(C)C)N1C(C)=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a413f39439cd436fae92766aebf207f9
CI.CN(C)c1ccccc1CSC1=NC(=O)C(C)(C)N1>>CN1C(=O)C(C)(C)N=C1SCc1ccccc1N(C)C
CI.C(C)(=O)OCC.CN(C1=C(CSC=2NC(C(N2)=O)(C)C)C=CC=C1)C.[H-].[Na+]>>CN1C(=NC(C1=O)(C)C)SCC1=C(C=CC=C1)N(C)C
I[CH3:1].[N:2]1=[C:9]([S:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[N:18]([CH3:19])[CH3:20])[NH:8][C:5]([CH3:6])([CH3:7])[C:3]1=[O:4]>>[CH3:1][N:2]1[C:3](=[O:4])[C:5]([CH3:6])([CH3:7])[N:8]=[C:9]1[S:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][c:17]1[N:18]([CH3:19])[CH3:20]
CI.CN(C)c1ccccc1CSC1=NC(=O)C(C)(C)N1
CN1C(=O)C(C)(C)N=C1SCc1ccccc1N(C)C
null
null
CN(C=O)C.O
Heteroatom Alkylation and Arylation
OtherReaction
0be3157781bde9164f230f39a40e60ca4b3fb1f0c76158e8c5f3dfbca33c830f
4ba71d6749f69ee61012b6d9409145f900f668ab403cb291b681d5aeae64f724
O=C1CN=C(SCc2ccccc2)N1
I-[CH3;D1;+0:1].[C:2]-[#16:3]-[C;H0;D3;+0:4]1=[N;H0;D2;+0:5]-[C:6](=[O;D1;H0:7])-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[NH;D2;+0:11]-1>>[C:2]-[#16:3]-[C;H0;D3;+0:4]1=[N;H0;D2;+0:11]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C:6](=[O;D1;H0:7])-[N;H0;D3;+0:5]-1-[CH3;D1;+0:1]
null
[]
null
null
15
MINUTE
To a solution of 0.5 g of 2-(2-dimethylaminobenzylthio)-5,5-dimethylimidazolin-4-one in 20 mL of N,N-dimethylformamide, there was added 60% sodium hydride in 0.09 g of mineral oil at -10° C. After the mixture was stirred for 15 minutes, 1 mL of methyl iodide was added to the mixture, and the stirring was continued for ...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Monosulfide
Tertiary amide.Monosulfide
C1=NCCN1
C1=NCC[NH]1
C1=NCC[NH]1.c1ccccc1
HI
CN(C=O)C.O
null
0.25
CI.CN(C)c1ccccc1CSC1=NC(=O)C(C)(C)N1>CN(C=O)C.O>CN1C(=O)C(C)(C)N=C1SCc1ccccc1N(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-673e7e0da0374e52b0efea0bb7e74951
CC1(C)NC(=O)NC1=S.CN(C)c1ccccc1CCl>>CN(C)c1ccccc1CSC1=NC(=O)NC1(C)C
Cl.CN(C1=C(CCl)C=CC=C1)C.CC1(C(NC(N1)=O)=S)C>>CN(C1=C(CSC2=NC(NC2(C)C)=O)C=CC=C1)C
[S:11]=[C:12]1[NH:13][C:14](=[O:15])[NH:16][C:17]1([CH3:18])[CH3:19].Cl[CH2:10][c:9]1[c:4]([N:2]([CH3:1])[CH3:3])[cH:5][cH:6][cH:7][cH:8]1>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[CH2:10][S:11][C:12]1=[N:13][C:14](=[O:15])[NH:16][C:17]1([CH3:18])[CH3:19]
CC1(C)NC(=O)NC1=S.CN(C)c1ccccc1CCl
CN(C)c1ccccc1CSC1=NC(=O)NC1(C)C
null
null
CO
Protection
OtherReaction
9b3fffcd549d2c61072b189884f428b95bb57a9cdd6f96fd60fb385384688724
a0306b442dafb3274f3ed52a8c28cb63392109c07f21b1295aafb9782efd645c
O=C1N=C(SCc2ccccc2)CN1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C;D1;H3:5]-[C:6]1(-[C;D1;H3:7])-[#7:8]-[C:9](=[O;D1;H0:10])-[NH;D2;+0:11]-[C;H0;D3;+0:12]-1=[S;H0;D1;+0:13]>>[C;D1;H3:5]-[C:6]1(-[C;D1;H3:7])-[#7:8]-[C:9](=[O;D1;H0:10])-[N;H0;D2;+0:11]=[C;H0;D3;+0:12]-1-[S;H0;D2;+0:13]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
2
HOUR
Initially, 2.5 g of 2-dimethylaminobenzylchloride hydrochloride was added to a solution of 1.5 g of 5,5-dimethyl-4-thiohydantoin in 50 mL of methanol (MeQH). The reaction mixture was stirred for two hours at the room temperature and concentrated in vacuo. To the residue, there was added 100 mL of CHCl3. The residue was...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Urea.Thioamide
Monosulfide
C1CNCN1
C1=NCNC1
c1ccccc1.C1=NCNC1
HCl
CO
null
2
CC1(C)NC(=O)NC1=S.CN(C)c1ccccc1CCl>CO>CN(C)c1ccccc1CSC1=NC(=O)NC1(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-963943015c7a4df68483236ac94750d2
CI.CN(C)c1ccccc1CSC1=NC(=O)NC1(C)C>>CN(C)c1ccccc1CSC1=NC(=O)N(C)C1(C)C
CN(C1=C(CSC2=NC(NC2(C)C)=O)C=CC=C1)C.CI>>CN1C(N=C(C1(C)C)SCC1=C(C=CC=C1)N(C)C)=O
I[CH3:17].[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[CH2:10][S:11][C:12]1=[N:13][C:14](=[O:15])[NH:16][C:18]1([CH3:19])[CH3:20]>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[CH2:10][S:11][C:12]1=[N:13][C:14](=[O:15])[N:16]([CH3:17])[C:18]1([CH3:19])[CH3:20]
CI.CN(C)c1ccccc1CSC1=NC(=O)NC1(C)C
CN(C)c1ccccc1CSC1=NC(=O)N(C)C1(C)C
null
null
null
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
d5e3d23d7d875f5fef574aa8ac112f262bc116b9d0f20a791bb9059d51b12b58
0a16658309ac5595448433dd7ef49294830b145345df0b202ccd54727262e629
O=C1N=C(SCc2ccccc2)CN1
I-[CH3;D1;+0:1].[C;D1;H3:2]-[C:3]1(-[C;D1;H3:4])-[C:5]=[#7:6]-[C:7](=[O;D1;H0:8])-[NH;D2;+0:9]-1>>[C;D1;H3:2]-[C:3]1(-[C;D1;H3:4])-[C:5]=[#7:6]-[C:7](=[O;D1;H0:8])-[N;H0;D3;+0:9]-1-[CH3;D1;+0:1]
null
[]
null
null
null
null
Initially, 0.5 g of 4-(2-dimethylaminobenzylthio)-5,5-dimethyl-3-imidazolin-2-one was reacted with 1 mL of methyl iodide following the procedure used in Example 35. The desired compound was obtained in the form of a syrup. The yield of this compound was 0.43 g with a yield ratio of 81.9%. A result of a 1 H-NMR analysis...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
Tertiary amide
C1=NCNC1
C1=NC[NH]C1
c1ccccc1.C1=NC[NH]C1
HI
null
null
null
CI.CN(C)c1ccccc1CSC1=NC(=O)NC1(C)C>>CN(C)c1ccccc1CSC1=NC(=O)N(C)C1(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-7b3987398bb64abd9f359af3d6a7e88d
CCC1(C)NC(=O)NC1=S.CN(C)c1ccccc1CCl>>CCC1(C)NC(=O)N=C1SCc1ccccc1N(C)C
Cl.CN(C1=C(CCl)C=CC=C1)C.C(C)C1(C(NC(N1)=O)=S)C>>CN(C1=C(CSC2=NC(NC2(C)CC)=O)C=CC=C1)C
[CH3:1][CH2:2][C:3]1([CH3:4])[NH:5][C:6](=[O:7])[NH:8][C:9]1=[S:10].Cl[CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][c:17]1[N:18]([CH3:19])[CH3:20]>>[CH3:1][CH2:2][C:3]1([CH3:4])[NH:5][C:6](=[O:7])[N:8]=[C:9]1[S:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][c:17]1[N:18]([CH3:19])[CH3:20]
CCC1(C)NC(=O)NC1=S.CN(C)c1ccccc1CCl
CCC1(C)NC(=O)N=C1SCc1ccccc1N(C)C
null
null
null
Protection
OtherReaction
9b3fffcd549d2c61072b189884f428b95bb57a9cdd6f96fd60fb385384688724
a0306b442dafb3274f3ed52a8c28cb63392109c07f21b1295aafb9782efd645c
O=C1N=C(SCc2ccccc2)CN1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]1(-[C;D1;H3:7])-[#7:8]-[C:9](=[O;D1;H0:10])-[NH;D2;+0:11]-[C;H0;D3;+0:12]-1=[S;H0;D1;+0:13]>>[C:5]-[C:6]1(-[C;D1;H3:7])-[#7:8]-[C:9](=[O;D1;H0:10])-[N;H0;D2;+0:11]=[C;H0;D3;+0:12]-1-[S;H0;D2;+0:13]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
In the present Example, 2.3 g of 2-dimethylaminobenzylchloride hydrochloride and 1.5 g of 5-ethyl-5-methyl-4-thiohydantoin were reacted following the procedure used in Example 36. Crystallization from diethyl ether-n-hexane gave the desired compound in the form of a needle-like crystal. The yield of this compound was 1...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Urea.Thioamide
Monosulfide
C1CNCN1
C1=NCNC1
C1=NCNC1.c1ccccc1
HCl
null
null
null
CCC1(C)NC(=O)NC1=S.CN(C)c1ccccc1CCl>>CCC1(C)NC(=O)N=C1SCc1ccccc1N(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a4c2572338d149fc9b4505fc6cb945cf
CC1(C)NC(=S)NC1=S.CN(C)c1ccccc1CCl>>CN(C)c1ccccc1CSC1=NC(C)(C)C(SCc2ccccc2N(C)C)=N1
Cl.CN(C1=C(CCl)C=CC=C1)C.CC1(C(NC(N1)=S)=S)C>>CN(C1=C(CSC2=NC(C(=N2)SCC2=C(C=CC=C2)N(C)C)(C)C)C=CC=C1)C
[NH:2]1[C:12](=[S:11])[NH:13][C:14]([CH3:15])([CH3:16])[C:17]1=[S:18].Cl[CH2:10][c:9]1[cH:8][cH:7][cH:23][cH:24][c:25]1[N:26]([CH3:1])[CH3:3]>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[CH2:10][S:11][C:12]1=[N:13][C:14]([CH3:15])([CH3:16])[C:17]([S:18][CH2:19][c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]2[N:...
CC1(C)NC(=S)NC1=S.CN(C)c1ccccc1CCl
CN(C)c1ccccc1CSC1=NC(C)(C)C(SCc2ccccc2N(C)C)=N1
null
null
C(C)O.CCO
Aromatic Heterocycle Formation
OtherReaction
e9e0dcb8157350c39f7294759583be48483c609eab6bad3b352b3679b60ba21a
e14cd4806f58873333c499a92a4f5dd98ee7ba7de93b394b5f309b7d3984cce3
c1ccc(CSC2=NC(SCc3ccccc3)=NC2)cc1
Cl-[CH2;D2;+0:1]-[c;H0;D3;+0:2]1:[c:3]:[cH;D2;+0:4]:[cH;D2;+0:5]:[c:6]:[c;H0;D3;+0:7]:1-[N;H0;D3;+0:8](-[CH3;D1;+0:9])-[CH3;D1;+0:10].[C;D1;H3:11]-[C:12]1(-[C;D1;H3:13])-[NH;D2;+0:14]-[C;H0;D3;+0:15](=[S;H0;D1;+0:16])-[NH;D2;+0:17]-[C;H0;D3;+0:18]-1=[S;H0;D1;+0:19]>>[C;D1;H3:11]-[C:12]1(-[C;D1;H3:13])-[N;H0;D2;+0:14]=[...
null
[]
null
null
1.5
HOUR
Initially, a solution of 9.1 g of 2-dimethylaminobenzylchloride hydrochloride in 50 mL of EtOH was added to a solution of 7 g of 5,5-dimethyl-2,4-dithiohydantoin in 100 mL of ethanol (EtOH). The reaction mixture was stirred for 1.5 hour at the room temperature and concentrated in vacuo. To the residue, there was added ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea.Thioamide.Tertiary amine
Tertiary amine.Tertiary amine.Monosulfide.Monosulfide
C1CNCN1.c1ccccc1
c1ccccc1.C1=NC=NC1.c1ccccc1
c1ccccc1.C1=NC=NC1.c1ccccc1
null
C(C)O.CCO
null
1.5
CC1(C)NC(=S)NC1=S.CN(C)c1ccccc1CCl>C(C)O.CCO>CN(C)c1ccccc1CSC1=NC(C)(C)C(SCc2ccccc2N(C)C)=N1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5666a9282ea5444b92b3aab759b61587
CC1(C)NC(=S)NC1=S.CN(C)c1ccccc1CCl>>CN(C)c1ccccc1CSC1=NC(=S)C(C)(C)N1
Cl.CN(C1=C(CCl)C=CC=C1)C.CC1(C(NC(N1)=S)=S)C>>CN(C1=C(CSC=2NC(C(N2)=S)(C)C)C=CC=C1)C
[S:11]=[C:12]1[NH:13][C:14](=[S:15])[C:16]([CH3:17])([CH3:18])[NH:19]1.Cl[CH2:10][c:9]1[c:4]([N:2]([CH3:1])[CH3:3])[cH:5][cH:6][cH:7][cH:8]1>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[CH2:10][S:11][C:12]1=[N:13][C:14](=[S:15])[C:16]([CH3:17])([CH3:18])[NH:19]1
CC1(C)NC(=S)NC1=S.CN(C)c1ccccc1CCl
CN(C)c1ccccc1CSC1=NC(=S)C(C)(C)N1
null
null
C(Cl)(Cl)Cl
Protection
OtherReaction
46cef1e48600fcd6705529550ccb17b294e17c854f6cacd0473e52ed0910cca7
f72dba6c0cce6a796ff9aeda8637cc446706f96a34b889e05557c4a922c09746
S=C1CNC(SCc2ccccc2)=N1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C:6]1-[C:7]-[#7:8]-[C;H0;D3;+0:9](=[S;H0;D1;+0:10])-[NH;D2;+0:11]-1>>[S;D1;H0:5]=[C:6]1-[C:7]-[#7:8]-[C;H0;D3;+0:9](-[S;H0;D2;+0:10]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])=[N;H0;D2;+0:11]-1
null
[]
null
null
30
MINUTE
Initially, 11 g of 2-dimethylaminobenzylchloride hydrochloride was added to a solution of 8 g of 5,5-dimethyl-2,4-dithiohydantoin in 200 mL of chloroform (CHCl3) at about 60° C. The reaction mixture was stirred for 30 minutes and washed with an aqueous solution of NaHCO3, dried over MgSO4, and concentrated in vacuo. Th...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea
Monosulfide
C1CNCN1
C1=NCCN1
c1ccccc1.C1=NCCN1
HCl
C(Cl)(Cl)Cl
null
0.5
CC1(C)NC(=S)NC1=S.CN(C)c1ccccc1CCl>C(Cl)(Cl)Cl>CN(C)c1ccccc1CSC1=NC(=S)C(C)(C)N1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-dc25bdb7c4ad482f819d561626b78d70
CC1(C)NC(=S)NC1=S.ClCc1ccccn1>>CC1(C)NC(SCc2ccccn2)=NC1=S
Cl.ClCC1=NC=CC=C1.CC1(C(NC(N1)=S)=S)C.[OH-].[Na+]>>N1=C(C=CC=C1)CSC=1NC(C(N1)=S)(C)C
[CH3:1][C:2]1([CH3:3])[NH:4][C:5](=[S:6])[NH:14][C:15]1=[S:16].Cl[CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][n:13]1>>[CH3:1][C:2]1([CH3:3])[NH:4][C:5]([S:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][n:13]2)=[N:14][C:15]1=[S:16]
CC1(C)NC(=S)NC1=S.ClCc1ccccn1
CC1(C)NC(SCc2ccccn2)=NC1=S
null
null
null
Protection
OtherReaction
46cef1e48600fcd6705529550ccb17b294e17c854f6cacd0473e52ed0910cca7
f72dba6c0cce6a796ff9aeda8637cc446706f96a34b889e05557c4a922c09746
S=C1CNC(SCc2ccccn2)=N1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[S;D1;H0:6]=[C:7]1-[C:8]-[#7:9]-[C;H0;D3;+0:10](=[S;H0;D1;+0:11])-[NH;D2;+0:12]-1>>[S;D1;H0:6]=[C:7]1-[C:8]-[#7:9]-[C;H0;D3;+0:10](-[S;H0;D2;+0:11]-[CH2;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5])=[N;H0;D2;+0:12]-1
null
[]
null
null
1
HOUR
Initially, 2.7 g of 2-chloromethylpyridine hydrochloride was added to a solution of 2.4g of 5,5-dimethyl-2,4-dithiohydantoin in 17 mL of 2N aqueous solution of NaOH. The reaction mixture was stirred for one hour at the room temperature, and extracted with 100 mL of chloroform (CHCl3). The CHCl3 layer was dried over MgS...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea
Monosulfide
C1CNCN1
C1=NCCN1
C1=NCCN1.c1ccncc1
HCl
null
null
1
CC1(C)NC(=S)NC1=S.ClCc1ccccn1>>CC1(C)NC(SCc2ccccn2)=NC1=S
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-483dd6c046dd4bfda158d9c42f0f2afc
CC1(C)NC(=S)NC1=S.CN(C)c1cccc(CCl)c1>>CN(C)c1cccc(CSC2=NC(C)(C)C(SCc3cccc(N(C)C)c3)=N2)c1
Cl.CN(C=1C=C(CCl)C=CC1)C.CC1(C(NC(N1)=S)=S)C.C[O-].[Na+]>>CN(C=1C=C(CSC2=NC(C(=N2)SCC2=CC(=CC=C2)N(C)C)(C)C)C=CC1)C
[NH:2]1[C:11](=[S:10])[NH:28][C:16](=[S:17])[C:13]1([CH3:14])[CH3:15].Cl[CH2:18][c:19]1[cH:20][cH:21][cH:22][c:23]([N:24]([CH3:1])[CH3:3])[cH:27]1>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][c:8]([CH2:9][S:10][C:11]2=[N:12][C:13]([CH3:14])([CH3:15])[C:16]([S:17][CH2:18][c:19]3[cH:20][cH:21][cH:22][c:23]([N:24]([CH3:...
CC1(C)NC(=S)NC1=S.CN(C)c1cccc(CCl)c1
CN(C)c1cccc(CSC2=NC(C)(C)C(SCc3cccc(N(C)C)c3)=N2)c1
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
0a28fd05626e226c3e61952969504b1e7c751e2809b3309b230576220ee1b0a7
e14cd4806f58873333c499a92a4f5dd98ee7ba7de93b394b5f309b7d3984cce3
c1ccc(CSC2=NC(SCc3ccccc3)=NC2)cc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[c:5](-[N;H0;D3;+0:6](-[CH3;D1;+0:7])-[CH3;D1;+0:8]):[c:9].[C;D1;H3:10]-[C;H0;D4;+0:11]1(-[C;D1;H3:12])-[NH;D2;+0:13]-[C;H0;D3;+0:14](=[S;H0;D1;+0:15])-[NH;D2;+0:16]-[C;H0;D3;+0:17]-1=[S;H0;D1;+0:18]>>[C;D1;H3:10]-[C;H0;D4;+0:11]1(-[C;D1;H3:12])-[#7:19]=[C;H0;D3;+0:14](-[S;H0;D2;+0:...
null
[]
null
null
1
HOUR
Initially, 2.94 g of 3-dimethylaminobenzylchloride hydrochloride was added to a mixture of 1.6 g of 5,5-dimethyl-2,4-dithiohydantoin and 1.3 g of sodium methoxide in 50 mL of methanol (MeOH). The reaction mixture was stirred at the room temperature for one hour, and concentrated in vacuo. The residue was treated follow...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea.Thioamide.Tertiary amine
Tertiary amine.Tertiary amine.Monosulfide.Monosulfide
C1CNCN1
c1ccccc1.C1=NC=NC1
c1ccccc1.C1=NC=NC1.c1ccccc1
null
CO
null
1
CC1(C)NC(=S)NC1=S.CN(C)c1cccc(CCl)c1>CO>CN(C)c1cccc(CSC2=NC(C)(C)C(SCc3cccc(N(C)C)c3)=N2)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a4efbc932fc544199dcb61e6467fceea
BrCc1cccc2cccnc12.CC1(C)NC(=S)NC1=S>>CC1(C)N=C(SCc2cccc3cccnc23)N=C1SCc1cccc2cccnc12
BrCC=1C=CC=C2C=CC=NC12.CC1(C(NC(N1)=S)=S)C>>N1=CC=CC2=CC=CC(=C12)CSC1=NC(C(=N1)SCC=1C=CC=C2C=CC=NC12)(C)C
Br[CH2:7][c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][cH:14][cH:15][n:16][c:17]12.[CH3:1][C:2]1([CH3:27])[NH:4][C:5](=[S:6])[NH:18][C:19]1=[S:20]>>[CH3:1][C:2]1([CH3:3])[N:4]=[C:5]([S:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][cH:14][cH:15][n:16][c:17]23)[N:18]=[C:19]1[S:20][CH2:21][c:22]1[cH:23][cH:24][cH:25][c:26]...
BrCc1cccc2cccnc12.CC1(C)NC(=S)NC1=S
CC1(C)N=C(SCc2cccc3cccnc23)N=C1SCc1cccc2cccnc12
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
02d24859d5480827ffc30869aaf0794e217b6a931fcfe10e3ee2647b9a0cbcbf
99e12b03eade0fe69501b6a285a6b4a4c50012c54f35269925bc496acff18eb3
c1cnc2c(CSC3=NC(SCc4cccc5cccnc45)=NC3)cccc2c1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7].[C;D1;H3:8]-[C;H0;D4;+0:9]1(-[CH3;D1;+0:10])-[NH;D2;+0:11]-[C;H0;D3;+0:12](=[S;H0;D1;+0:13])-[NH;D2;+0:14]-[C;H0;D3;+0:15]-1=[S;H0;D1;+0:16]>>[C;D1;H3:8]-[C;H0;D4;+0:9]1(-[C;D1;H3:17])-[N;H0;D2;+0:11]=[C;H0;D3;+0:12](-[S;H0;D2;+0:13]-[CH2;D2;+0:1]-[c:2](:[c:3]...
null
[]
null
null
1.5
HOUR
Initially, 3 g of 8-bromomethylquinoline was added to a solution of 1 g of 5,5-dimethyl-2,4-dithiohydantoin in 50 mL of ethanol (EtOH). The reaction mixture was stirred at the room temperature for 1.5 hour, and concentrated in vacuo. To the residue, 100 mL of CHCl3 was added. The mixture was washed with an aqueous solu...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea.Thioamide
Monosulfide.Monosulfide
C1CNCN1
C1=NC=NC1.c1ccc2ncccc2c1
C1=NC=NC1.c1ccc2ncccc2c1.c1ccc2ncccc2c1
Br-
C(C)O
null
1.5
BrCc1cccc2cccnc12.CC1(C)NC(=S)NC1=S>C(C)O>CC1(C)N=C(SCc2cccc3cccnc23)N=C1SCc1cccc2cccnc12
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1ddb24d2ec1c4eb5b7c0603a217b4d61
CC1(C)NC(=S)NC1=S.CN(C)c1cccc(CCl)c1>>CN(C)c1cccc(CSC2=NC(C)(C)C(SCc3cccc(N(C)C)c3)=N2)c1
Cl.CN(C=1C=C(CCl)C=CC1)C.CC1(C(NC(N1)=S)=S)C.C[O-].[Na+]>>CN(C=1C=C(CSC2=NC(C(=N2)SCC2=CC(=CC=C2)N(C)C)(C)C)C=CC1)C
[NH:2]1[C:11](=[S:10])[NH:28][C:16](=[S:17])[C:13]1([CH3:14])[CH3:15].Cl[CH2:18][c:19]1[cH:20][cH:21][cH:22][c:23]([N:24]([CH3:1])[CH3:3])[cH:27]1>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][c:8]([CH2:9][S:10][C:11]2=[N:12][C:13]([CH3:14])([CH3:15])[C:16]([S:17][CH2:18][c:19]3[cH:20][cH:21][cH:22][c:23]([N:24]([CH3:...
CC1(C)NC(=S)NC1=S.CN(C)c1cccc(CCl)c1
CN(C)c1cccc(CSC2=NC(C)(C)C(SCc3cccc(N(C)C)c3)=N2)c1
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
0a28fd05626e226c3e61952969504b1e7c751e2809b3309b230576220ee1b0a7
e14cd4806f58873333c499a92a4f5dd98ee7ba7de93b394b5f309b7d3984cce3
c1ccc(CSC2=NC(SCc3ccccc3)=NC2)cc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[c:5](-[N;H0;D3;+0:6](-[CH3;D1;+0:7])-[CH3;D1;+0:8]):[c:9].[C;D1;H3:10]-[C;H0;D4;+0:11]1(-[C;D1;H3:12])-[NH;D2;+0:13]-[C;H0;D3;+0:14](=[S;H0;D1;+0:15])-[NH;D2;+0:16]-[C;H0;D3;+0:17]-1=[S;H0;D1;+0:18]>>[C;D1;H3:10]-[C;H0;D4;+0:11]1(-[C;D1;H3:12])-[#7:19]=[C;H0;D3;+0:14](-[S;H0;D2;+0:...
null
[]
null
null
null
null
Initially, 3.1 g of 3-dimethylaminobenzylchloride hydrochloride was added to a mixture of 0.8 g of 5,5-dimethyl-2,4-dithiohydantoin and 1.34 g of sodium methoxide in 50 mL of methanol (MeOH). The reaction mixture was treated following the procedure used in Example 56, and purified by column chromatograph (CHCl3) to giv...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea.Thioamide.Tertiary amine
Tertiary amine.Tertiary amine.Monosulfide.Monosulfide
C1CNCN1
c1ccccc1.C1=NC=NC1
c1ccccc1.C1=NC=NC1.c1ccccc1
null
CO
null
null
CC1(C)NC(=S)NC1=S.CN(C)c1cccc(CCl)c1>CO>CN(C)c1cccc(CSC2=NC(C)(C)C(SCc3cccc(N(C)C)c3)=N2)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6f30ba70e6f749ca9b50c7fefb87d362
CC1(C)NC(=S)NC1=S.CN(C)c1ccc(CCl)cc1>>CN(C)c1ccc(CSC2=NC(C)(C)C(SCc3ccc(N(C)C)cc3)=N2)cc1
Cl.CN(C1=CC=C(CCl)C=C1)C.CC1(C(NC(N1)=S)=S)C>>CN(C1=CC=C(CSC2=NC(C(=N2)SCC2=CC=C(C=C2)N(C)C)(C)C)C=C1)C
[NH:2]1[C:10](=[S:9])[NH:27][C:15](=[S:16])[C:12]1([CH3:13])[CH3:18].Cl[CH2:8][c:7]1[cH:6][cH:25][c:21]([N:22]([CH3:1])[CH3:3])[cH:29][cH:28]1>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([CH2:8][S:9][C:10]2=[N:11][C:12]([CH3:13])([CH3:14])[C:15]([S:16][CH2:17][c:18]3[cH:19][cH:20][c:21]([N:22]([CH3:23])[CH3:24])[cH:2...
CC1(C)NC(=S)NC1=S.CN(C)c1ccc(CCl)cc1
CN(C)c1ccc(CSC2=NC(C)(C)C(SCc3ccc(N(C)C)cc3)=N2)cc1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
e9e0dcb8157350c39f7294759583be48483c609eab6bad3b352b3679b60ba21a
e14cd4806f58873333c499a92a4f5dd98ee7ba7de93b394b5f309b7d3984cce3
c1ccc(CSC2=NC(SCc3ccccc3)=NC2)cc1
Cl-[CH2;D2;+0:1]-[c:2]1:[c:3]:[cH;D2;+0:4]:[c;H0;D3;+0:5](-[N;H0;D3;+0:6](-[CH3;D1;+0:7])-[CH3;D1;+0:8]):[cH;D2;+0:9]:[cH;D2;+0:10]:1.[C;D1;H3:11]-[C;H0;D4;+0:12]1(-[CH3;D1;+0:13])-[NH;D2;+0:14]-[C;H0;D3;+0:15](=[S;H0;D1;+0:16])-[NH;D2;+0:17]-[C;H0;D3;+0:18]-1=[S;H0;D1;+0:19]>>[C;D1;H3:11]-[C;H0;D4;+0:12]1(-[C;D1;H3:20...
null
[]
null
null
null
null
Initially, 3.2 g of 4-dimethylaminobenzylchloride hydrochloride was added to a solution of 1 g of 5,5-dimethyl-2,4-dithiohydantoin in 50 mL of ethanol (EtOH). The reaction mixture was treated following the procedure used in Example 62, and purified by column chromatography (CHCl3). Recrystallization form diethyl ether-...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea.Thioamide.Tertiary amine
Tertiary amine.Tertiary amine.Monosulfide.Monosulfide
C1CNCN1.c1ccccc1
c1ccccc1.C1=NC=NC1.c1ccccc1
c1ccccc1.C1=NC=NC1.c1ccccc1
null
C(C)O
null
null
CC1(C)NC(=S)NC1=S.CN(C)c1ccc(CCl)cc1>C(C)O>CN(C)c1ccc(CSC2=NC(C)(C)C(SCc3ccc(N(C)C)cc3)=N2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2f49fa4e191649188ac77496c1af416a
BrCc1ccccc1.CC1(C)NC(=S)NC1=S>>CC1(C)NC(SCc2ccccc2)=NC1=S
C(C1=CC=CC=C1)Br.CC1(C(NC(N1)=S)=S)C>>C(C1=CC=CC=C1)SC=1NC(C(N1)=S)(C)C
Br[CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1.[CH3:1][C:2]1([CH3:3])[NH:4][C:5](=[S:6])[NH:14][C:15]1=[S:16]>>[CH3:1][C:2]1([CH3:3])[NH:4][C:5]([S:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)=[N:14][C:15]1=[S:16]
BrCc1ccccc1.CC1(C)NC(=S)NC1=S
CC1(C)NC(SCc2ccccc2)=NC1=S
null
null
C(C)O
Protection
OtherReaction
46cef1e48600fcd6705529550ccb17b294e17c854f6cacd0473e52ed0910cca7
f72dba6c0cce6a796ff9aeda8637cc446706f96a34b889e05557c4a922c09746
S=C1CNC(SCc2ccccc2)=N1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C:6]1-[C:7]-[#7:8]-[C;H0;D3;+0:9](=[S;H0;D1;+0:10])-[NH;D2;+0:11]-1>>[S;D1;H0:5]=[C:6]1-[C:7]-[#7:8]-[C;H0;D3;+0:9](-[S;H0;D2;+0:10]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])=[N;H0;D2;+0:11]-1
null
[]
null
null
1
HOUR
Initially, 1.91 mL of benzylbromide was added to a solution of 1.6 g of 5,5-dimethyl-2,4-dithiohydantoin in 50 mL of ethanol (EtOH). The reaction mixture was stirred at the room temperature for one hour, and concentrated in vacuo. The residue was treated following the procedure used in Example 62, and purified by colum...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea
Monosulfide
C1CNCN1
C1=NCCN1
C1=NCCN1.c1ccccc1
HBr
C(C)O
null
1
BrCc1ccccc1.CC1(C)NC(=S)NC1=S>C(C)O>CC1(C)NC(SCc2ccccc2)=NC1=S
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9a24f90cc7884da083a28d124bc01ed8
CC1(C)NC(SCc2ccccc2)=NC1=S.CN(C)c1ccccc1CCl>>CN(C)c1ccccc1CSC1=NC(SCc2ccccc2)=NC1(C)C
Cl.CN(C1=C(CCl)C=CC=C1)C.C(C1=CC=CC=C1)SC=1NC(C(N1)=S)(C)C>>C(C1=CC=CC=C1)SC1=NC(C(=N1)SCC1=C(C=CC=C1)N(C)C)(C)C
[S:11]=[C:12]1[N:13]=[C:14]([S:15][CH2:16][c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[NH:23][C:24]1([CH3:25])[CH3:26].Cl[CH2:10][c:9]1[c:4]([N:2]([CH3:1])[CH3:3])[cH:5][cH:6][cH:7][cH:8]1>>[CH3:1][N:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:8][c:9]1[CH2:10][S:11][C:12]1=[N:13][C:14]([S:15][CH2:16][c:17]2[cH:18][cH:19][cH...
CC1(C)NC(SCc2ccccc2)=NC1=S.CN(C)c1ccccc1CCl
CN(C)c1ccccc1CSC1=NC(SCc2ccccc2)=NC1(C)C
null
null
C(C)O
Protection
OtherReaction
2cae177f6d4ae1a04201a67501987621d8d2eea3bcb1c5c3e45f226cf8eb2595
73c8878a4ec89c98dabc6fa1f37724ccebee7c1f418fd0d5ec558cb2e2ee1385
c1ccc(CSC2=NC(SCc3ccccc3)=NC2)cc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[#16:6]-[C;H0;D3;+0:7]1=[N;H0;D2;+0:8]-[C;H0;D3;+0:9](=[S;H0;D1;+0:10])-[C:11](-[C;D1;H3:12])(-[C;D1;H3:13])-[NH;D2;+0:14]-1>>[C:5]-[#16:6]-[C;H0;D3;+0:7]1=[N;H0;D2;+0:14]-[C:11](-[C;D1;H3:12])(-[C;D1;H3:13])-[C;H0;D3;+0:9](-[S;H0;D2;+0:10]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])=[...
null
[]
null
null
1
HOUR
Initially, 0.65 g of 2-dimethylaminobenzylchloride hydrochloride was added to a solution of 0.7 g of 2-benzylthio-5,5-dimethylimidazolin-4-thione in 20 mL of ethanol (EtOH). The reaction mixture was stirred at the room temperature for one hour, and concentrated in vacuo. The residue was treated following the procedure ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine.Monosulfide
Monosulfide.Monosulfide
C1=NCCN1
C1=NC=NC1
c1ccccc1.C1=NC=NC1.c1ccccc1
HCl
C(C)O
null
1
CC1(C)NC(SCc2ccccc2)=NC1=S.CN(C)c1ccccc1CCl>C(C)O>CN(C)c1ccccc1CSC1=NC(SCc2ccccc2)=NC1(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f8004c340bcb48f79c38943b43d382ec
COc1ccc(C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c(SSc2cc(OC)ccc2C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c1>>COc1ccc(C(=O)NC(CC(C)C)C(=O)O)c(SSc2cc(OC)ccc2C(=O)NC(CC(C)C)C(=O)O)c1
C1(=CC=CC=C1)C.C(C)(C)(C)OC(C(CC(C)C)NC(C1=C(C=C(C=C1)OC)SSC1=C(C=CC(=C1)OC)C(NC(CC(C)C)C(=O)OC(C)(C)C)=O)=O)=O.C1(=CC=CC=C1)OC.FC(C(=O)O)(F)F>>C(=O)(O)C(CC(C)C)NC(=O)C1=C(C=C(C=C1)OC)SSC1=C(C(=O)NC(C(=O)O)CC(C)C)C=CC(=C1)OC
CC(C)(C)[O:17][C:15]([CH:10]([NH:9][C:7]([c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:40][c:18]1[S:19][S:20][c:21]1[cH:22][c:23]([O:24][CH3:25])[cH:26][cH:27][c:28]1[C:29](=[O:30])[NH:31][CH:32]([CH2:33][CH:34]([CH3:35])[CH3:36])[C:37](=[O:38])[O:39]C(C)(C)C)=[O:8])[CH2:11][CH:12]([CH3:13])[CH3:14])=[O:16]>>[CH3:1][O:2][c:...
COc1ccc(C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c(SSc2cc(OC)ccc2C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c1
COc1ccc(C(=O)NC(CC(C)C)C(=O)O)c(SSc2cc(OC)ccc2C(=O)NC(CC(C)C)C(=O)O)c1
null
null
ClCCl
Deprotection
OtherReaction
ca505900a12db9f5b5e9f03319157f3a1866191dca0d7b3ac3055953edad48a1
6963b6f47a0b0b5cff914a710e9b301204a20bd63f6727c47e40cb3bb5699806
c1ccc(SSc2ccccc2)cc1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].C-C(-C)(-C)-[O;H0;D2;+0:5]-[C:6](-[C:7])=[O;D1;H0:8]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1].[C:7]-[C:6](=[O;D1;H0:8])-[OH;D1;+0:5]
69.5
[{"value": 69.5, "product": "C(=O)(O)C(CC(C)C)NC(=O)C1=C(C=C(C=C1)OC)SSC1=C(C(=O)NC(C(=O)O)CC(C)C)C=CC(=C1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
A solution of [S-(R*,R*)-2[2-[2-(1-tert-butoxycarbonyl-3-methyl-butylcarbamoyl)-5-methoxyphenyldisulfanyl]-4-methoxybenzoylamino]-4-methyl-pentanoic acid tert-butyl ester (1.2 g, 1.7 mmol) and anisole (1 mL) in 10 mL dichloromethane, cooled to about 0° C., was treated dropwise with 10 mL of trifluoroacetic acid. The mi...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Boc.Boc
Carboxylic acid.Carboxylic acid
null
null
c1ccccc1.c1ccccc1
Other
ClCCl
null
4
COc1ccc(C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c(SSc2cc(OC)ccc2C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c1>ClCCl>COc1ccc(C(=O)NC(CC(C)C)C(=O)O)c(SSc2cc(OC)ccc2C(=O)NC(CC(C)C)C(=O)O)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-119962b494b84a6c9cbee5d7dffaf002
CC(C)CC(NC(=O)c1cc(F)ccc1SSN(C(=O)c1cccc(F)c1)C(CC(C)C)C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>CC(C)CC(NC(=O)c1cc(F)ccc1SSc1ccc(F)cc1C(=O)NC(CC(C)C)C(=O)O)C(=O)O
C(C)(C)(C)OC(C(CC(C)C)N(C(C1=CC=CC(=C1)F)=O)SSC1=C(C=C(C=C1)F)C(NC(CC(C)C)C(=O)OC(C)(C)C)=O)=O.FC(C(=O)O)(F)F>>C(=O)(O)C(CC(C)C)NC(=O)C1=C(C=CC(=C1)F)SSC1=C(C(=O)NC(C(=O)O)CC(C)C)C=C(C=C1)F
CC(C)(C)[O:35][C:33]([CH:28]([N:27]([S:17][S:16][c:15]1[c:9]([C:7]([NH:6][CH:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[C:36](=[O:37])[O:38]C(C)(C)C)=[O:8])[cH:10][c:11]([F:12])[cH:13][cH:14]1)[C:25]([c:24]1[cH:18][cH:19][cH:20][c:21]([F:22])[cH:23]1)=[O:26])[CH2:29][CH:30]([CH3:31])[CH3:32])=[O:34]>>[CH3:1][CH:2]([CH3:3])[CH2:...
CC(C)CC(NC(=O)c1cc(F)ccc1SSN(C(=O)c1cccc(F)c1)C(CC(C)C)C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
CC(C)CC(NC(=O)c1cc(F)ccc1SSc1ccc(F)cc1C(=O)NC(CC(C)C)C(=O)O)C(=O)O
null
null
ClCCl.C1(=CC=CC=C1)OC
Miscellaneous
OtherReaction
09c4d392b48c016291b6d1ce537fb29e14ce0694d0a924f483700fcd8f1e3231
6001f211511fe6682852bbd6a1d306f30447f74f772ed9de084e37d61a5abdd7
c1ccc(SSc2ccccc2)cc1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].C-C(-C)(-C)-[O;H0;D2;+0:5]-[C:6](=[O;D1;H0:7])-[C:8](-[C:9])-[N;H0;D3;+0:10](-[S;H0;D2;+0:11]-[#16:12]-[c:13])-[C:14](=[O;D1;H0:15])-[c:16](:[c:17]):[cH;D2;+0:18]:[c:19]:[c:20]>>[C:9]-[C:8](-[NH;D2;+0:10]-[C:14](=[O;D1;H0:15])-[c:16](:[c:17]):[c;H0;D3;+0:18](-[S;H0;D...
null
[]
null
null
null
null
The general method of Preparation 20 was followed using [S-(R*,R*)]-2-[2-[[2-(1-tert-butoxycarbonyl-3-methyl-butylcarbamoyl)-4-fluorophenyldisulfanyl]-5-fluorobenzoylamino]-4-methyl pentanoic acid tert-butyl ester (1.8 g, 2.6 mmol) in 20 mL dichloromethane, anisole (2 mL), and 20 mL trifluoroacetic acid. The crude prod...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Tertiary amide.Disulfide.Boc.Boc
Carboxylic acid.Carboxylic acid.Secondary amide.Disulfide
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
Other
ClCCl.C1(=CC=CC=C1)OC
null
null
CC(C)CC(NC(=O)c1cc(F)ccc1SSN(C(=O)c1cccc(F)c1)C(CC(C)C)C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>ClCCl.C1(=CC=CC=C1)OC>CC(C)CC(NC(=O)c1cc(F)ccc1SSc1ccc(F)cc1C(=O)NC(CC(C)C)C(=O)O)C(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-30c9c4c43e504a87b22ef5a3d62b32e8
Cc1ccc(C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c(SSc2cc(C)ccc2C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c1>>Cc1cccc([SH](Sc2cc(C)ccc2C(=O)NC(CC(C)C)C(=O)O)C(=O)NC(CC(C)C)C(=O)O)c1
C(C)(C)(C)OC(C(CC(C)C)NC(C1=C(C=C(C=C1)C)SSC1=C(C=CC(=C1)C)C(NC(CC(C)C)C(=O)OC(C)(C)C)=O)=O)=O.FC(C(=O)O)(F)F>>C(=O)(O)C(CC(C)C)NC(=O)S(SC1=C(C(=O)NC(C(=O)O)CC(C)C)C=CC(=C1)C)C1=CC=CC(=C1)C
CC(C)(C)[O:26][C:24]([CH:19]([NH:18][C:16]([c:15]1[c:9]([S:8][S:7][c:6]2[c:5]([C:27](=[O:28])[NH:29][CH:30]([CH2:31][CH:32]([CH3:33])[CH3:34])[C:35](=[O:36])[O:37]C(C)(C)C)[cH:4][cH:3][c:2]([CH3:1])[cH:38]2)[cH:10][c:11]([CH3:12])[cH:13][cH:14]1)=[O:17])[CH2:20][CH:21]([CH3:22])[CH3:23])=[O:25]>>[CH3:1][c:2]1[cH:3][cH:...
Cc1ccc(C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c(SSc2cc(C)ccc2C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c1
Cc1cccc([SH](Sc2cc(C)ccc2C(=O)NC(CC(C)C)C(=O)O)C(=O)NC(CC(C)C)C(=O)O)c1
null
null
ClCCl.C1(=CC=CC=C1)OC
Miscellaneous
OtherReaction
97cc7ca54c3504cdddd49cbb6f307a3515c6323edeca45fe75deed785c490c73
d55bea45c3105c0907c3b9459dc25f38e24a2cb4199f6499f0844204a38592ad
c1ccc(SSc2ccccc2)cc1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].C-C(-C)(-C)-[O;H0;D2;+0:5]-[C:6](=[O;D1;H0:7])-[C:8]-[#7:9]-[C;H0;D3;+0:10](=[O;D1;H0:11])-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15](-[S;H0;D2;+0:16]-[#16:17]-[c:18]):[c:19]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1].[O;D1;H0:11]=[C;H0;D3;+0:10](-[#7:9]-[C:8]-[C:6](=[O;D1;...
null
[]
null
null
null
null
The general method of Preparation 20 was followed using [S-(R*,R*)]-2-[2-[2-(1-tert-butoxycarbonyl-3-methyl-butylcarbamoyl)-5-methyl-phenyldisulfanyl]-4-methyl-benzoylamino]-4-methyl-pentanoic acid tert-butyl ester (1.9 g, 2.8 mmol) in 20 mL dichloromethane, anisole (2.0 mL), and 10 mL trifluoroacetic acid. The crude p...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Secondary amide.Disulfide.Boc.Boc
Carboxylic acid.Carboxylic acid.Secondary amide
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
Other
ClCCl.C1(=CC=CC=C1)OC
null
null
Cc1ccc(C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c(SSc2cc(C)ccc2C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)c1>ClCCl.C1(=CC=CC=C1)OC>Cc1cccc([SH](Sc2cc(C)ccc2C(=O)NC(CC(C)C)C(=O)O)C(=O)NC(CC(C)C)C(=O)O)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1e43db34740c4500b323da3d86603bf8
CC(C)CC(NC(=O)c1cccnc1SSc1ncccc1C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>CC(C)CC(NC(=O)c1cccnc1SSc1ncccc1C(=O)NC(CC(C)C)C(=O)O)C(=O)O
C(C)(C)(C)OC(C(CC(C)C)NC(=O)C=1C(=NC=CC1)SSC1=NC=CC=C1C(NC(CC(C)C)C(=O)OC(C)(C)C)=O)=O.FC(C(=O)O)(F)F>>C(=O)(O)C(CC(C)C)NC(=O)C=1C(=NC=CC1)SSC1=NC=CC=C1C(=O)NC(C(=O)O)CC(C)C
CC(C)(C)[O:33][C:31]([CH:26]([NH:25][C:23]([c:22]1[c:17]([S:16][S:15][c:14]2[c:9]([C:7]([NH:6][CH:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[C:34](=[O:35])[O:36]C(C)(C)C)=[O:8])[cH:10][cH:11][cH:12][n:13]2)[n:18][cH:19][cH:20][cH:21]1)=[O:24])[CH2:27][CH:28]([CH3:29])[CH3:30])=[O:32]>>[CH3:1][CH:2]([CH3:3])[CH2:4][CH:5]([NH:6][...
CC(C)CC(NC(=O)c1cccnc1SSc1ncccc1C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
CC(C)CC(NC(=O)c1cccnc1SSc1ncccc1C(=O)NC(CC(C)C)C(=O)O)C(=O)O
null
null
ClCCl.C1(=CC=CC=C1)OC
Deprotection
OtherReaction
ca505900a12db9f5b5e9f03319157f3a1866191dca0d7b3ac3055953edad48a1
6963b6f47a0b0b5cff914a710e9b301204a20bd63f6727c47e40cb3bb5699806
c1ccc(SSc2ccccn2)nc1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4].C-C(-C)(-C)-[O;H0;D2;+0:5]-[C:6](-[C:7])=[O;D1;H0:8]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1].[C:7]-[C:6](=[O;D1;H0:8])-[OH;D1;+0:5]
77.4
[{"value": 77.4, "product": "C(=O)(O)C(CC(C)C)NC(=O)C=1C(=NC=CC1)SSC1=NC=CC=C1C(=O)NC(C(=O)O)CC(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The general method of Preparation 20 was followed using [S-(R*,R*)]-2-([2-[3-(1-tert-butoxycarbonyl-3-methyl-butylcarbamoyl)-pyridin-2-yldisulfanyl]pyridine-3-carbonyl]-amino)-4-methyl-pentanoic acid tert-butyl ester (1.9 g, 2.9 mmol) in 20 mL dichloromethane, anisole (1.5 mL), and 10 mL trifluoroacetic acid. The crude...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Boc.Boc
Carboxylic acid.Carboxylic acid
null
null
c1ccncc1.c1ccncc1
Other
ClCCl.C1(=CC=CC=C1)OC
null
null
CC(C)CC(NC(=O)c1cccnc1SSc1ncccc1C(=O)NC(CC(C)C)C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>ClCCl.C1(=CC=CC=C1)OC>CC(C)CC(NC(=O)c1cccnc1SSc1ncccc1C(=O)NC(CC(C)C)C(=O)O)C(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-669072172d11414b8d8b946fb369fa91
O=C(O)c1cc([N+](=O)[O-])ccc1Cl>>NC(=O)c1cc([N+](=O)[O-])ccc1Cl
CN(C=O)C.ClC1=C(C(=O)O)C=C(C=C1)[N+](=O)[O-].ClCCl.C(C(=O)Cl)(=O)Cl>>ClC1=C(C(=O)N)C=C(C=C1)[N+](=O)[O-]
O[C:2](=[O:3])[c:4]1[cH:5][c:6]([N+:7](=[O:8])[O-:9])[cH:10][cH:11][c:12]1[Cl:13]>>[NH2:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([N+:7](=[O:8])[O-:9])[cH:10][cH:11][c:12]1[Cl:13]
O=C(O)c1cc([N+](=O)[O-])ccc1Cl
NC(=O)c1cc([N+](=O)[O-])ccc1Cl
null
null
null
Functional Group Interconversion
OtherReaction
e1b1a1f71ee10336b9e90a021457b106dbfe08a22161aaad6804675a8134a46f
5d384be3554a01fd49be5eb779c3b10075a4cc9a2373eb20aaa867286d4e28a9
c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]>>[N;D1;H2:6]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
null
[]
25
CELSIUS
3
HOUR
A mixture of 2-chloro-5-nitrobenzoic acid (15.0 g, 74.0 mmol) and 200 mL of dichloromethane was reacted with oxalyl chloride (16.2 mL, 186.0 mmol) and a catalytic amount of dimethylformamide. The mixture was stirred at 25° C. for 3 hours. The solvent was removed in vacuo, and the residue was redissolved in 200 mL of di...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary amide
null
null
c1ccccc1
null
null
25
3
O=C(O)c1cc([N+](=O)[O-])ccc1Cl>>NC(=O)c1cc([N+](=O)[O-])ccc1Cl
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-31a8839874394a4985cf9f31ccc798f0
NC(=O)c1cc([N+](=O)[O-])ccc1SSc1ccc([N+](=O)[O-])cc1C(N)=O>>NC(=O)c1cc(N)ccc1SSc1ccc(N)cc1C(N)=O
[OH-].[Na+].[N+](=O)([O-])C=1C=CC(=C(C(=O)N)C1)SSC1=C(C(=O)N)C=C(C=C1)[N+](=O)[O-].C(C)(=O)O>>NC=1C=CC(=C(C(=O)N)C1)SSC1=C(C(=O)N)C=C(C=C1)N
O=[N+:7]([O-])[c:6]1[cH:5][c:4]([C:2]([NH2:1])=[O:3])[c:10]([S:11][S:12][c:13]2[cH:14][cH:15][c:16]([N+:17](=O)[O-])[cH:18][c:19]2[C:20]([NH2:21])=[O:22])[cH:9][cH:8]1>>[NH2:1][C:2](=[O:3])[c:4]1[cH:5][c:6]([NH2:7])[cH:8][cH:9][c:10]1[S:11][S:12][c:13]1[cH:14][cH:15][c:16]([NH2:17])[cH:18][c:19]1[C:20]([NH2:21])=[O:22]
NC(=O)c1cc([N+](=O)[O-])ccc1SSc1ccc([N+](=O)[O-])cc1C(N)=O
NC(=O)c1cc(N)ccc1SSc1ccc(N)cc1C(N)=O
null
null
O
Reduction
OtherReaction
6748a51a25102225412593c5a930e43f5a8904a80803177de025a6f83c59d65e
a303b0dfb15cc6bade463acf71681cf3ba7580b599dfa4d28d8caac83d08cd17
c1ccc(SSc2ccccc2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4].O=[N+;H0;D3:5](-[O-])-[c:6](:[c:7]):[c:8]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]
null
[]
null
null
null
null
2,2'-Dithiobis(5-nitrobenzamide) (2.6 g, 7.0 mmol) was added portion-wise to a refluxing slurry of reduced iron (8.7 g) in 65 mL of water containing 0.1 mL of acetic acid. The resulting slurry was heated at reflux for 2.0 hours, then cooled to room temperature. The slurry was made strongly basic (pH 11) by the addition...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Nitro group
Primary amine.Primary amine
null
null
c1ccccc1.c1ccccc1
Other
O
null
null
NC(=O)c1cc([N+](=O)[O-])ccc1SSc1ccc([N+](=O)[O-])cc1C(N)=O>O>NC(=O)c1cc(N)ccc1SSc1ccc(N)cc1C(N)=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c2c072d6e317473092782f2fc460da4e
CC(=O)NS(=O)(=O)c1ccc(N)cc1.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl>>CC(=O)NS(=O)(=O)c1ccc(NC(=O)c2ccccc2SSc2ccccc2C(=O)Nc2ccc(S(=O)(=O)NC(C)=O)cc2)cc1
C(C1=C(C=CC=C1)SSC1=C(C(=O)Cl)C=CC=C1)(=O)Cl.C(C)(=O)NS(=O)(=O)C1=CC=C(N)C=C1>>C(C)(=O)NS(=O)(=O)C1=CC=C(C=C1)NC(C1=C(C=CC=C1)SSC1=C(C(=O)NC2=CC=C(C=C2)S(=O)(=O)NC(C)=O)C=CC=C1)=O
[CH3:1][C:2](=[O:3])[NH:4][S:5](=[O:6])(=[O:7])[c:8]1[cH:9][cH:10][c:11]([NH2:12])[cH:45][cH:46]1.Cl[C:29]([c:28]1[c:23]([S:22][S:21][c:20]2[cH:15][cH:13][cH:17][cH:16][c:41]2[C:40](Cl)=[O:42])[cH:24][cH:25][cH:26][cH:27]1)=[O:30]>>[CH3:1][C:2](=[O:3])[NH:4][S:5](=[O:6])(=[O:7])[c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=...
CC(=O)NS(=O)(=O)c1ccc(N)cc1.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl
CC(=O)NS(=O)(=O)c1ccc(NC(=O)c2ccccc2SSc2ccccc2C(=O)Nc2ccc(S(=O)(=O)NC(C)=O)cc2)cc1
null
null
ClCCl.N1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
22cd1dc72a4041b0ef5b7db292b4184290c99b70de74a0aed5aa6007b828688f
01a9fdf9dcb9d81e0891ccaaf29dcc22bb434a60fd36ce79777612cbb6766e1f
O=C(Nc1ccccc1)c1ccccc1SSc1ccccc1C(=O)Nc1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]-[#16:6]-[#16:7]-[c;H0;D3;+0:8]1:[cH;D2;+0:9]:[cH;D2;+0:10]:[cH;D2;+0:11]:[cH;D2;+0:12]:[c;H0;D3;+0:13]:1-[C;H0;D3;+0:14](-Cl)=[O;D1;H0:15].[NH2;D1;+0:16]-[c:17](:[c:18]):[c:19]>>[#16:20]-[#7:21]-[C;H0;D3;+0:14](-[CH3;D1;+0:13])=[O;D1;H0:15].[O;D1;H0:22]=[C;H0;D3;+0:10...
8.9
[{"value": 8.9, "product": "C(C)(=O)NS(=O)(=O)C1=CC=C(C=C1)NC(C1=C(C=CC=C1)SSC1=C(C(=O)NC2=CC=C(C=C2)S(=O)(=O)NC(C)=O)C=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The compound was prepared according to the general method of Preparation 9 using 2,2'-dithiobisbenzoyl chloride (3.0 g, 8.0 mmol) in 30 mL of dichloromethane and 4-[(acetylamino) sulfonyl]aniline (5.6 g, 26.0 mmol) in 100 mL of pyridine. The crude product was purified on a silica gel column using chloroform/methanol (1...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Primary amine
Sulfonamide.Secondary amide.Secondary amide.Secondary amide
c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
null
ClCCl.N1=CC=CC=C1
null
null
CC(=O)NS(=O)(=O)c1ccc(N)cc1.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl>ClCCl.N1=CC=CC=C1>CC(=O)NS(=O)(=O)c1ccc(NC(=O)c2ccccc2SSc2ccccc2C(=O)Nc2ccc(S(=O)(=O)NC(C)=O)cc2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-93e8df1342c5499d9b84345b5640a0a8
CC(C)[C@H](N)C(=O)O.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl>>CC(C)C(NC(=O)c1ccccc1SSc1ccccc1C(=O)NC(C(=O)O)C(C)C)C(=O)O
N[C@@H](C(C)C)C(=O)O.C(C1=C(C=CC=C1)SSC1=C(C(=O)Cl)C=CC=C1)(=O)Cl>>C(=O)(O)C(C(C)C)NC(=O)C1=C(C=CC=C1)SSC1=C(C(=O)NC(C(=O)O)C(C)C)C=CC=C1
[CH3:1][CH:2]([C@H:4]([NH2:5])[C:32](=[O:33])[OH:34])[CH3:22].Cl[C:6](=[O:7])[c:8]1[cH:9][cH:10][cH:11][cH:12][c:13]1[S:14][S:15][c:16]1[cH:17][cH:18][cH:19][cH:20][c:25]1[C:26](Cl)=[O:23]>>[CH3:1][CH:2]([CH3:3])[CH:4]([NH:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][cH:11][cH:12][c:13]1[S:14][S:15][c:16]1[cH:17][cH:18][cH:19][c...
CC(C)[C@H](N)C(=O)O.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl
CC(C)C(NC(=O)c1ccccc1SSc1ccccc1C(=O)NC(C(=O)O)C(C)C)C(=O)O
null
null
null
Acylation
OtherReaction
96aec30bc29f8a10c5a9c59dd38293a9e70242b09892d1cb15e88bd21ee48682
562f98a770adee9ece495a4b94774feb5cfb15c943140651fe293450590314a5
c1ccc(SSc2ccccc2)cc1
Cl-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c;H0;D3;+0:3]1:[cH;D2;+0:4]:[c:5]:[c:6]:[c:7]:[c;H0;D3;+0:8]:1-[#16:9]-[#16:10]-[c:11]:[c:12](-[C;H0;D3;+0:13](-Cl)=[O;D1;H0:14]):[c:15].[C;D1;H3:16]-[CH;D3;+0:17](-[CH3;D1;+0:18])-[C@H;D3;+0:19](-[NH2;D1;+0:20])-[C:21](=[O;D1;H0:22])-[O;D1;H1:23]>>[C;D1;H3:16]-[CH;D3;+0:17](-[C;D1;H...
null
[]
null
null
null
null
Using the method employed in Preparation 30, 17.8 g (0.15 mol) of D,L valine was reacted with 17.2 g (0.05 mol) of 2,2'-dithiobisbenzoyl chloride to produce 11.4 g of the title compound after recrystallization from acetic acid, mp 226.5°-227.5° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Primary amine
Carboxylic acid.Secondary amide.Secondary amide
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
null
null
null
null
CC(C)[C@H](N)C(=O)O.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl>>CC(C)C(NC(=O)c1ccccc1SSc1ccccc1C(=O)NC(C(=O)O)C(C)C)C(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-22175d52cf8d4bbdad038a1e70ab65ca
NCCCC(=O)O.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl>>O=C(O)CCCNC(=O)c1ccccc1SSc1ccccc1C(=O)NCCCC(=O)O
NCCCC(=O)O.C(C1=C(C=CC=C1)SSC1=C(C(=O)Cl)C=CC=C1)(=O)Cl>>C(=O)(O)CCCNC(=O)C1=C(C=CC=C1)SSC1=C(C(=O)NCCCC(=O)O)C=CC=C1
[C:2](=[O:3])([CH2:4][CH2:5][CH2:6][NH2:7])[OH:32].Cl[C:8](=[O:9])[c:10]1[cH:11][cH:12][cH:13][cH:14][c:15]1[S:16][S:17][c:18]1[cH:19][cH:29][cH:28][cH:27][c:23]1[C:24](Cl)=[O:1]>>[O:1]=[C:2]([OH:3])[CH2:4][CH2:5][CH2:6][NH:7][C:8](=[O:9])[c:10]1[cH:11][cH:12][cH:13][cH:14][c:15]1[S:16][S:17][c:18]1[cH:19][cH:20][cH:21...
NCCCC(=O)O.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl
O=C(O)CCCNC(=O)c1ccccc1SSc1ccccc1C(=O)NCCCC(=O)O
null
null
null
C-C Coupling
OtherReaction
d181252499baa49109ed23d54d62027be0aa3b7f5e994ef4d92e4bdf0a015f68
a985834843373a464595eec57cb32af1587b5397fe48448982dd54839413def7
c1ccc(SSc2ccccc2)cc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].Cl-[C;H0;D3;+0:6](=[O;H0;D1;+0:7])-[c;H0;D3;+0:8]1:[cH;D2;+0:9]:[cH;D2;+0:10]:[cH;D2;+0:11]:[cH;D2;+0:12]:[c:13]:1-[#16:14].[NH2;D1;+0:15]-[C:16]-[C:17]-[C:18]-[C;H0;D3;+0:19](=[O;H0;D1;+0:20])-[OH;D1;+0:21]>>[#16:14]-[c:13]1:[cH;D2;+0:12]:[c:22]:[c:23]:[c:24]:[c;H0;D...
49.9
[{"value": 49.9, "product": "C(=O)(O)CCCNC(=O)C1=C(C=CC=C1)SSC1=C(C(=O)NCCCC(=O)O)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure in Preparation 30, 16 g (0.15 mol) of 4-amino-butanoic acid was reacted with 10.8 g (0.03 mol) of 2,2'-dithiobisbenzoyl chloride to afford 7.14 g of the title compound. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Carboxylic acid.Primary amine
Carboxylic acid.Carboxylic acid.Secondary amide.Secondary amide
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
null
null
null
null
NCCCC(=O)O.O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl>>O=C(O)CCCNC(=O)c1ccccc1SSc1ccccc1C(=O)NCCCC(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4a1716f3e5114ac89523fbe7390dee6c
CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1Cl.S>>CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1S
C(C)N(CCNC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)Cl)CC.S.[Na]>>C(C)N(CCNC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S)CC
Cl[c:22]1[c:11]([C:9]([NH:8][CH2:7][CH2:6][N:3]([CH2:2][CH3:1])[CH2:4][CH3:5])=[O:10])[cH:12][n:13][c:14](-[c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[n:21]1.[SH2:23]>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][NH:8][C:9](=[O:10])[c:11]1[cH:12][n:13][c:14](-[c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[n:21][c:2...
CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1Cl.S
CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1S
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
070c5e407a5456f15b44a24a4a55d2593c0b85e22043fab594367ab9ef8d8c3e
5acfc94bcb91f90cc14ddd9f791d64cf2f45381ebe181eac63cc3d2843bb00cd
c1ccc(-c2ncccn2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[c:4]):[#7;a:5]:[c:6]:[c:7]:1-[C:8](=[O;D1;H0:9])-[#7:10]-[C:11].[SH2;D0;+0:12]>>[C:11]-[#7:10]-[C:8](=[O;D1;H0:9])-[c:7]1:[c:6]:[#7;a:5]:[c:3](-[c:4]):[#7;a:2]:[c;H0;D3;+0:1]:1-[SH;D1;+0:12]
63.6
[{"value": 63.6, "product": "C(C)N(CCNC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure in Preparation 34, 6.4 g (0.02 mol) of 4-chloro-2-phenyl-pyrimidine-5-carboxylic acid (2-diethylamino-ethyl)-amide was reacted with 4.8 g (0.066 mol) of sodium hydrogen sulfide to afford 4.2 g of the title compound, mp 178°-180° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Aromatic thiol
c1cncnc1
c1cncnc1
c1cncnc1.c1ccccc1
HCl
null
null
null
CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1Cl.S>>CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1S
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1bfad829bc4246f8aaa002d4fbd32d86
CN(C)c1ncc(C(=O)NCc2ccccc2)c(Cl)n1.S>>CN(C)c1ncc(C(=O)NCc2ccccc2)c(S)n1
C(C1=CC=CC=C1)NC(=O)C=1C(=NC(=NC1)N(C)C)Cl.S.[Na]>>C(C1=CC=CC=C1)NC(=O)C=1C(=NC(=NC1)N(C)C)S
Cl[c:18]1[c:7]([C:8](=[O:9])[NH:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[cH:6][n:5][c:4]([N:2]([CH3:1])[CH3:3])[n:20]1.[SH2:19]>>[CH3:1][N:2]([CH3:3])[c:4]1[n:5][cH:6][c:7]([C:8](=[O:9])[NH:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[c:18]([SH:19])[n:20]1
CN(C)c1ncc(C(=O)NCc2ccccc2)c(Cl)n1.S
CN(C)c1ncc(C(=O)NCc2ccccc2)c(S)n1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
070c5e407a5456f15b44a24a4a55d2593c0b85e22043fab594367ab9ef8d8c3e
5acfc94bcb91f90cc14ddd9f791d64cf2f45381ebe181eac63cc3d2843bb00cd
O=C(NCc1ccccc1)c1cncnc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[#7:4]):[#7;a:5]:[c:6]:[c:7]:1-[C:8](=[O;D1;H0:9])-[#7:10]-[C:11].[SH2;D0;+0:12]>>[#7:4]-[c:3]1:[#7;a:2]:[c;H0;D3;+0:1](-[SH;D1;+0:12]):[c:7](-[C:8](=[O;D1;H0:9])-[#7:10]-[C:11]):[c:6]:[#7;a:5]:1
43.9
[{"value": 43.9, "product": "C(C1=CC=CC=C1)NC(=O)C=1C(=NC(=NC1)N(C)C)S", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Preparation 34, 14.3 g (0.045 mol) of 4-chloro-2-dimethylamino-pyrimidine-5-carboxylic acid benzylamide and 12 g (0.21 mol) of sodium hydrogen sulfide were reacted to give 5.7 g of the title compound, mp 175°-178° C. Conditions: See reaction.notes.procedure_details. Workup: were reacted
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Aromatic thiol
c1cncnc1
c1cncnc1
c1cncnc1.c1ccccc1
HCl
null
null
null
CN(C)c1ncc(C(=O)NCc2ccccc2)c(Cl)n1.S>>CN(C)c1ncc(C(=O)NCc2ccccc2)c(S)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-73bd32edf0dc4454ae0af2e0d20af183
O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1Cl.S>>O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1S
C(C1=CC=CC=C1)NC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)Cl.S.[Na]>>C(C1=CC=CC=C1)NC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S
Cl[c:22]1[c:11]([C:2](=[O:1])[NH:3][CH2:4][c:5]2[cH:6][cH:7][cH:8][cH:9][cH:10]2)[cH:12][n:13][c:14](-[c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[n:21]1.[SH2:23]>>[O:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[c:11]1[cH:12][n:13][c:14](-[c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[n:21][c:22]1[SH:23]
O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1Cl.S
O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1S
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
070c5e407a5456f15b44a24a4a55d2593c0b85e22043fab594367ab9ef8d8c3e
5acfc94bcb91f90cc14ddd9f791d64cf2f45381ebe181eac63cc3d2843bb00cd
O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[c:4]):[#7;a:5]:[c:6]:[c:7]:1-[C:8](=[O;D1;H0:9])-[#7:10]-[C:11].[SH2;D0;+0:12]>>[C:11]-[#7:10]-[C:8](=[O;D1;H0:9])-[c:7]1:[c:6]:[#7;a:5]:[c:3](-[c:4]):[#7;a:2]:[c;H0;D3;+0:1]:1-[SH;D1;+0:12]
65.2
[{"value": 65.2, "product": "C(C1=CC=CC=C1)NC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure from Preparation 34, 5.8 g (17.9 mmol) of 4-chloro-2-phenyl-pyrimidine-5-carboxylic acid benzylamide was reacted with 5.1 g (72 mmol) of sodium hydrogen sulfide to give 3.75 g of the title compound, mp 189°-193° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Aromatic thiol
c1cncnc1
c1cncnc1
c1ccccc1.c1cncnc1.c1ccccc1
HCl
null
null
null
O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1Cl.S>>O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1S
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4067666dc2a34bd280d72f658a8ab4f7
CCC(C)C(NC(=O)c1ccccc1C(=O)N(SSc1ccccc1)C(C(=O)O)C(C)CC)C(=O)O>>CCC(C)C(C(=O)O)n1sc2ccccc2c1=O
C(=O)(O)C(C(CC)C)NC(=O)C1=C(C(=O)N(C(C(=O)O)C(CC)C)SSC2=CC=CC=C2)C=CC=C1.BrBr>>CC(C(C(=O)O)N1SC2=C(C1=O)C=CC=C2)CC
CCC(C)C(NC(=O)[c:11]1[cH:12][cH:13][cH:14][cH:15][c:16]1[C:17]([N:9]([CH:5]([CH:3]([CH2:2][CH3:1])[CH3:4])[C:6](=[O:7])[OH:8])[S:10]Sc1ccccc1)=[O:18])C(=O)O>>[CH3:1][CH2:2][CH:3]([CH3:4])[CH:5]([C:6](=[O:7])[OH:8])[n:9]1[s:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[c:17]1=[O:18]
CCC(C)C(NC(=O)c1ccccc1C(=O)N(SSc1ccccc1)C(C(=O)O)C(C)CC)C(=O)O
CCC(C)C(C(=O)O)n1sc2ccccc2c1=O
null
null
ClCCl
Miscellaneous
OtherReaction
e2926d905a02e34c58aa119038113df327a8b0c9b951a9c6c07d2367edb1d58e
95efc4ecf4ace74c5432ec55a35221782e607c11c8e2bcb5f206d10c974b4c9d
O=c1[nH]sc2ccccc12
C-C-C(-C)-C(-N-C(=O)-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C;H0;D3;+0:5](=[O;D1;H0:6])-[N;H0;D3;+0:7](-[S;H0;D2;+0:8]-S-c1:c:c:c:c:c:1)-[C:9](-[C:10])-[C:11](=[O;D1;H0:12])-[O;D1;H1:13]):[c:14])-C(-O)=O>>[C:10]-[C:9](-[C:11](=[O;D1;H0:12])-[O;D1;H1:13])-[n;H0;D3;+0:7]1:[s;H0;D2;+0:8]:[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](:...
null
[]
null
null
2
HOUR
To a stirred suspension of 5.3 g (10.0 mmol) of [S-(R*,R*)]-2-[2-[2-(1-carboxy-2-methylbutylcarbamoyl) phenyldisulfanylbenzoylamino]-3-methylpentanoic acid (from Preparation 19) in 200 mL of dichloromethane was added dropwise 2.4 g (15.0 mmol) of liquid bromine. The reaction mixture was stirred at room temperature for ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amide.Tertiary amide.Disulfide
null
c1ccccc1.c1ccccc1
c1ccc2sncc2c1
c1ccc2sncc2c1
Other
ClCCl
null
2
CCC(C)C(NC(=O)c1ccccc1C(=O)N(SSc1ccccc1)C(C(=O)O)C(C)CC)C(=O)O>ClCCl>CCC(C)C(C(=O)O)n1sc2ccccc2c1=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0793e59e7ec647808746d733896f2b78
CC(C)CC(NC(=O)c1cc(F)ccc1SSN(C(=O)c1cccc(F)c1)C(CC(C)C)C(=O)O)C(=O)O>>CC(C)C[C@@H](C(=O)O)n1sc2ccc(F)cc2c1=O
C(=O)(O)C(CC(C)C)NC(=O)C1=C(C=CC(=C1)F)SSN(C(C(=O)O)CC(C)C)C(C1=CC=CC(=C1)F)=O.BrBr>>CC(C[C@@H](C(=O)O)N1SC2=C(C1=O)C=C(C=C2)F)C
CC(C)CC(C(=O)O)N(S[S:10][c:11]1[cH:12][cH:13][c:14]([F:15])[cH:16][c:17]1[C:18]([NH:9][CH:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[C:6](=[O:7])[OH:8])=[O:19])C(=O)c1cccc(F)c1>>[CH3:1][CH:2]([CH3:3])[CH2:4][C@@H:5]([C:6](=[O:7])[OH:8])[n:9]1[s:10][c:11]2[cH:12][cH:13][c:14]([F:15])[cH:16][c:17]2[c:18]1=[O:19]
CC(C)CC(NC(=O)c1cc(F)ccc1SSN(C(=O)c1cccc(F)c1)C(CC(C)C)C(=O)O)C(=O)O
CC(C)C[C@@H](C(=O)O)n1sc2ccc(F)cc2c1=O
null
null
C(C)#N.ClCCl
Functional Group Interconversion
OtherReaction
76bf87ae358ee0e4e582cc211ac6dce89f9be7272cf4d3f440d8e6109870eedb
4b1cb94b9bd3f930196129229de6ede3f354bb1dc0c097c3268db81c49624c65
O=c1[nH]sc2ccccc12
C-C(-C)-C-C(-C(-O)=O)-N(-S-[S;H0;D2;+0:1]-[c:2](:[c:3]):[c:4](-[C;H0;D3;+0:5](=[O;D1;H0:6])-[NH;D2;+0:7]-[CH;D3;+0:8](-[C:9]-[C:10])-[C:11](=[O;D1;H0:12])-[O;D1;H1:13]):[c:14])-C(=O)-c1:c:c:c:c(-F):c:1>>[C:10]-[C:9]-[C@@H;D3;+0:8](-[C:11](=[O;D1;H0:12])-[O;D1;H1:13])-[n;H0;D3;+0:7]1:[s;H0;D2;+0:1]:[c:2](:[c:3]):[c:4](:...
137.3
[{"value": 137.3, "product": "CC(C[C@@H](C(=O)O)N1SC2=C(C1=O)C=C(C=C2)F)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the general method of Example 3, a slurry of {s-(R*,R*)]-2-{-[2-(1-carboxy-3-methylbutylcarbamoyl)-4-fluorophenyldisulfanyl]-5-fluorobenzoylamino}-4-methyl-pentanoic acid (2.1 g, 3.6 mmol) (from Preparation 21) in 8 mL acetonitrile and 25 mL dichloromethane was treated with bromine (0.7 g, 4.4 mmol) in 15 mL ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carboxylic acid.Secondary amide.Tertiary amide.Disulfide
null
c1ccccc1.c1ccccc1
c1ccc2sncc2c1
c1ccc2sncc2c1
HF
C(C)#N.ClCCl
null
null
CC(C)CC(NC(=O)c1cc(F)ccc1SSN(C(=O)c1cccc(F)c1)C(CC(C)C)C(=O)O)C(=O)O>C(C)#N.ClCCl>CC(C)C[C@@H](C(=O)O)n1sc2ccc(F)cc2c1=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6ee8845e6af847a2859d929ed8e2b575
Cc1cccc(C(=O)N(SSc2ccc(C)cc2C(=O)NC(CC(C)C)C(=O)O)C(CC(C)C)C(=O)O)c1>>Cc1ccc2c(=O)n([C@@H](CC(C)C)C(=O)O)sc2c1
C(=O)(O)C(CC(C)C)NC(=O)C1=C(C=CC(=C1)C)SSN(C(C(=O)O)CC(C)C)C(C1=CC=CC(=C1)C)=O.BrBr.C(C)#N>>CC(C[C@@H](C(=O)O)N1SC2=C(C1=O)C=CC(=C2)C)C
Cc1cccc(C(=O)N(S[S:17][c:18]2[cH:4][cH:3][c:2]([CH3:1])[cH:19][c:5]2[C:6](=[O:7])[NH:8][CH:9]([CH2:10][CH:11]([CH3:12])[CH3:13])[C:14](=[O:15])[OH:16])C(CC(C)C)C(=O)O)c1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[c:6](=[O:7])[n:8]([C@@H:9]([CH2:10][CH:11]([CH3:12])[CH3:13])[C:14](=[O:15])[OH:16])[s:17][c:18]2[cH:19]1
Cc1cccc(C(=O)N(SSc2ccc(C)cc2C(=O)NC(CC(C)C)C(=O)O)C(CC(C)C)C(=O)O)c1
Cc1ccc2c(=O)n([C@@H](CC(C)C)C(=O)O)sc2c1
null
null
ClCCl
Miscellaneous
OtherReaction
e2926d905a02e34c58aa119038113df327a8b0c9b951a9c6c07d2367edb1d58e
95efc4ecf4ace74c5432ec55a35221782e607c11c8e2bcb5f206d10c974b4c9d
O=c1[nH]sc2ccccc12
C-C(-C)-C-C(-C(-O)=O)-N(-S-[S;H0;D2;+0:1]-[c;H0;D3;+0:2]1:[cH;D2;+0:3]:[c:4]:[c:5](-[C;D1;H3:6]):[cH;D2;+0:7]:[c;H0;D3;+0:8]:1-[C;H0;D3;+0:9](=[O;D1;H0:10])-[NH;D2;+0:11]-[CH;D3;+0:12](-[C:13]-[C:14])-[C:15](=[O;D1;H0:16])-[O;D1;H1:17])-C(=O)-c1:c:c:c:c(-C):c:1>>[C:14]-[C:13]-[C@@H;D3;+0:12](-[C:15](=[O;D1;H0:16])-[O;D...
null
[]
null
null
null
null
Following the general method of Example 3, a slurry of [s-(R*,R*)]-2-[-[2-(1-carboxy-3-methylbutylcarbamoyl)-4-methylphenyldisulfanyl]-5-methylbenzoylamino]-4-methyl-pentanoic acid (1.8 g, 3.2 mmol) (from Preparation 22) in 5 mL acetonitrile and 20 mL dichloromethane was reacted with bromine (0.6 g, 3.7 mmol) in 10 mL ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amide.Tertiary amide.Disulfide
null
c1ccccc1.c1ccccc1
c1ccc2sncc2c1
c1ccc2sncc2c1
Other
ClCCl
null
null
Cc1cccc(C(=O)N(SSc2ccc(C)cc2C(=O)NC(CC(C)C)C(=O)O)C(CC(C)C)C(=O)O)c1>ClCCl>Cc1ccc2c(=O)n([C@@H](CC(C)C)C(=O)O)sc2c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c22db2c5c35e41f08e3017072fa1182e
CC(C)CC(NC(=O)c1ccccc1SSc1ccccc1C(=O)NC(C(=O)O)C(C)C)C(=O)O>>CC(C)C(C(=O)O)n1sc2ccccc2c1=O
C(=O)(O)C(CC(C)C)NC(=O)C1=C(C=CC=C1)SSC1=C(C(=O)NC(C(=O)O)C(C)C)C=CC=C1.BrBr>>CC(C(C(=O)O)N1SC2=C(C1=O)C=CC=C2)C
CC(C)CC(NC(=O)c1ccccc1S[S:9][c:10]1[cH:11][cH:12][cH:13][cH:14][c:15]1[C:16]([NH:8][CH:4]([CH:2]([CH3:1])[CH3:3])[C:5](=[O:6])[OH:7])=[O:17])C(=O)O>>[CH3:1][CH:2]([CH3:3])[CH:4]([C:5](=[O:6])[OH:7])[n:8]1[s:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1=[O:17]
CC(C)CC(NC(=O)c1ccccc1SSc1ccccc1C(=O)NC(C(=O)O)C(C)C)C(=O)O
CC(C)C(C(=O)O)n1sc2ccccc2c1=O
null
null
null
Functional Group Interconversion
OtherReaction
0da1c302bf8994aa4fa64122a299c748e0825162a15b81dbc8c678803311ec95
9dd1e9ea00940727b8b4f2806b324bac3e6ef39570802956483a80b59e367fa2
O=c1[nH]sc2ccccc12
C-C(-C)-C-C(-N-C(=O)-c1:c:c:c:c:c:1-S-[S;H0;D2;+0:1]-[c:2](:[c:3]):[c:4](-[C;H0;D3;+0:5](=[O;D1;H0:6])-[NH;D2;+0:7]-[C:8](-[C:9])-[C:10](=[O;D1;H0:11])-[O;D1;H1:12]):[c:13])-C(-O)=O>>[C:9]-[C:8](-[C:10](=[O;D1;H0:11])-[O;D1;H1:12])-[n;H0;D3;+0:7]1:[s;H0;D2;+0:1]:[c:2](:[c:3]):[c:4](:[c:13]):[c;H0;D3;+0:5]:1=[O;D1;H0:6]
0.1
[{"value": 0.1, "product": "CC(C(C(=O)O)N1SC2=C(C1=O)C=CC=C2)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Following the procedure of Example 13, 6.0 g (13.6 mol) of 2-[2-[2-(1-carboxy-3-methylbutyl carbamoyl)phenyldisulfanyl]benzoylamino]-3-methylbutanoic acid was reacted with bromine to provide 2.25 g of the title compound, mp 166°-168° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amide.Secondary amide.Disulfide
null
c1ccccc1.c1ccccc1
c1ccc2sncc2c1
c1ccc2sncc2c1
Other
null
null
null
CC(C)CC(NC(=O)c1ccccc1SSc1ccccc1C(=O)NC(C(=O)O)C(C)C)C(=O)O>>CC(C)C(C(=O)O)n1sc2ccccc2c1=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9a3df734465742dfad570b95ad696165
Cc1ccnc(N)c1.O=C(Cl)c1ccccc1SCl>>Cc1ccnc(-n2sc3ccccc3c2=O)c1
NC1=NC=CC(=C1)C.ClSC1=C(C(=O)Cl)C=CC=C1>>CC1=CC(=NC=C1)N1SC2=C(C1=O)C=CC=C2
[CH3:1][c:2]1[cH:3][cH:4][n:5][c:6]([NH2:7])[cH:17]1.Cl[S:8][c:9]1[cH:10][cH:11][cH:12][cH:13][c:14]1[C:15](Cl)=[O:16]>>[CH3:1][c:2]1[cH:3][cH:4][n:5][c:6](-[n:7]2[s:8][c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[c:15]2=[O:16])[cH:17]1
Cc1ccnc(N)c1.O=C(Cl)c1ccccc1SCl
Cc1ccnc(-n2sc3ccccc3c2=O)c1
null
null
N1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
c34db5504b6723593932211c018846dbbfd64df4cc5099d5a4650ff0dff0cc55
0fba682bfb017234b2a9a0cddcd0a6c1cf200968add3d32ec4b8be184522b775
O=c1c2ccccc2sn1-c1ccccn1
Cl-[S;H0;D2;+0:1]-[c:2](:[c:3]):[c:4](-[C;H0;D3;+0:5](-Cl)=[O;D1;H0:6]):[c:7].[NH2;D1;+0:8]-[c;H0;D3;+0:9](:[#7;a:10]:[c:11]):[c:12]:[c:13]>>[O;D1;H0:6]=[c;H0;D3;+0:5]1:[c:4](:[c:7]):[c:2](:[c:3]):[s;H0;D2;+0:1]:[n;H0;D3;+0:8]:1-[c;H0;D3;+0:9](:[#7;a:10]:[c:11]):[c:12]:[c:13]
37.1
[{"value": 37.1, "product": "CC1=CC(=NC=C1)N1SC2=C(C1=O)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
null
null
Using the method of Fischer and Hurni (Arzneimittel Forsch., 1964;14:1301) 5.4 g (0.05 mol) of 2-amino-4-methylpyridine in 50 mL of pyridine at 10° C. was reacted with 10.3 g (0.05 mol) of 2-chlorosulfenylbenzoyl chloride. The mixture was heated to 50° C. and maintained at that temperature for 2 hours. The mixture was ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Monosulfide
null
c1ccccc1
c1ccc2sncc2c1
c1ccncc1.c1ccc2sncc2c1
HCl
N1=CC=CC=C1
50
null
Cc1ccnc(N)c1.O=C(Cl)c1ccccc1SCl>N1=CC=CC=C1>Cc1ccnc(-n2sc3ccccc3c2=O)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4b393218356b401fbefc98b26c343968
Nc1ccc(CC(=O)O)cc1.O=C(Cl)c1ccccc1SCl>>O=C(O)Cc1ccc(-n2sc3ccccc3c2=O)cc1
NC1=CC=C(C=C1)CC(=O)O.C(C)N(CC)CC.ClSC1=C(C(=O)Cl)C=CC=C1>>O=C1N(SC2=C1C=CC=C2)C2=CC=C(C=C2)CC(=O)O
[O:1]=[C:2]([OH:3])[CH2:4][c:5]1[cH:6][cH:7][c:8]([NH2:9])[cH:19][cH:20]1.Cl[S:10][c:11]1[cH:12][cH:13][cH:14][cH:15][c:16]1[C:17](Cl)=[O:18]>>[O:1]=[C:2]([OH:3])[CH2:4][c:5]1[cH:6][cH:7][c:8](-[n:9]2[s:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[c:17]2=[O:18])[cH:19][cH:20]1
Nc1ccc(CC(=O)O)cc1.O=C(Cl)c1ccccc1SCl
O=C(O)Cc1ccc(-n2sc3ccccc3c2=O)cc1
null
null
CCOCCO
Aromatic Heterocycle Formation
OtherReaction
c34db5504b6723593932211c018846dbbfd64df4cc5099d5a4650ff0dff0cc55
0fba682bfb017234b2a9a0cddcd0a6c1cf200968add3d32ec4b8be184522b775
O=c1c2ccccc2sn1-c1ccccc1
Cl-[S;H0;D2;+0:1]-[c:2](:[c:3]):[c:4](-[C;H0;D3;+0:5](-Cl)=[O;D1;H0:6]):[c:7].[NH2;D1;+0:8]-[c;H0;D3;+0:9](:[c:10]:[c:11]):[c:12]:[c:13]>>[O;D1;H0:6]=[c;H0;D3;+0:5]1:[c:4](:[c:7]):[c:2](:[c:3]):[s;H0;D2;+0:1]:[n;H0;D3;+0:8]:1-[c;H0;D3;+0:9](:[c:10]:[c:11]):[c:12]:[c:13]
69.4
[{"value": 69.4, "product": "O=C1N(SC2=C1C=CC=C2)C2=CC=C(C=C2)CC(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a mixture of 7.55 g (0.05 mol) of 4-aminophenylacetic acid and 15.15 g (0.15 mol) of triethylamine in 25 mL of ethyl cellosolve was added 10.3 g (0.05 mol) of 2-chlorosulfenylbenzoyl chloride (Arzneimittel Forsch., 1964;14:1301). The mixture was stirred at room temperature for 3 hours, concentrated in vacuo, and wat...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Monosulfide
null
c1ccccc1
c1ccc2sncc2c1
c1ccccc1.c1ccc2sncc2c1
HCl
CCOCCO
null
3
Nc1ccc(CC(=O)O)cc1.O=C(Cl)c1ccccc1SCl>CCOCCO>O=C(O)Cc1ccc(-n2sc3ccccc3c2=O)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-612c475449ba4056a49ab5f66bcc7953
O=C(NCCc1ccccn1)c1cnc2cc3c(cc2c1S)OCO3>>O=c1c2cnc3cc4c(cc3c2sn1CCc1ccccn1)OCO4
N1=C(C=CC=C1)CCNC(=O)C=1C=NC=2C=C3C(=CC2C1S)OCO3.C(C)N(CC)CC.II>>N1=C(C=CC=C1)CCN1SC2=C(C=NC=3C=C4C(=CC23)OCO4)C1=O
[O:1]=[C:2]([c:3]1[cH:4][n:5][c:6]2[cH:7][c:8]3[c:9]([cH:10][c:11]2[c:12]1[SH:13])[O:23][CH2:24][O:25]3)[NH:14][CH2:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][n:22]1>>[O:1]=[c:2]1[c:3]2[cH:4][n:5][c:6]3[cH:7][c:8]4[c:9]([cH:10][c:11]3[c:12]2[s:13][n:14]1[CH2:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][n:22]1)[O:...
O=C(NCCc1ccccn1)c1cnc2cc3c(cc2c1S)OCO3
O=c1c2cnc3cc4c(cc3c2sn1CCc1ccccn1)OCO4
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
1e253101091a8f64f2a51d3c4b1ecc40da62f3180df666e96348f00c187cd3e0
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cnc3cc4c(cc3c2sn1CCc1ccccn1)OCO4
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[c:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[c:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
83
[{"value": 83.0, "product": "N1=C(C=CC=C1)CCN1SC2=C(C=NC=3C=C4C(=CC23)OCO4)C1=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To 4.1 g (0.012 mol) of 8-mercapto-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2-yl-ethyl)-amide (from Preparation 34) and 5 mL (0.035 mol) of triethylamine in 750 mL of methanol was added 2.95 g (0.012 mol) of iodine in 100 mL of methanol. The mixture was heated at reflux for 2 hours, cooled, and then c...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cnc2cc3c(cc2c1)OCO3
c1nsc2c1cnc1cc3c(cc12)OCO3
c1ccncc1.c1nsc2c1cnc1cc3c(cc12)OCO3
null
CO
null
null
O=C(NCCc1ccccn1)c1cnc2cc3c(cc2c1S)OCO3>CO>O=c1c2cnc3cc4c(cc3c2sn1CCc1ccccn1)OCO4
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-930c4b70242b44ebba4db43c1eff2ea3
CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1S>>CCN(CC)CCn1sc2nc(-c3ccccc3)ncc2c1=O
C(C)N(CCNC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S)CC.II>>C(C)N(CCN1SC2=NC(=NC=C2C1=O)C1=CC=CC=C1)CC
[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][NH:8][C:22]([c:21]1[c:10]([SH:9])[n:11][c:12](-[c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[n:19][cH:20]1)=[O:23]>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[CH2:6][CH2:7][n:8]1[s:9][c:10]2[n:11][c:12](-[c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)[n:19][cH:20][c:21]2[c:22]1=[O...
CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1S
CCN(CC)CCn1sc2nc(-c3ccccc3)ncc2c1=O
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1[nH]sc2nc(-c3ccccc3)ncc12
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[#7;a:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
68.5
[{"value": 68.5, "product": "C(C)N(CCN1SC2=NC(=NC=C2C1=O)C1=CC=CC=C1)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 3.3 g (0.01 mol) of 4-mercapto-2-phenyl-pyrimidine-5-carboxylic acid (2-diethylamino-ethyl)-amide (from Preparation 36) and 2.54 g (0.01 mol) of iodine were reacted to give 2.25 g of the title compound after recrystallization from isopropanol, mp 106°-107° C. Conditions: See reaction....
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.c1ccccc1
null
null
null
null
CCN(CC)CCNC(=O)c1cnc(-c2ccccc2)nc1S>>CCN(CC)CCn1sc2nc(-c3ccccc3)ncc2c1=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2baa31474e604438bd652d473531a78e
O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1Cc1ccccc1
C(C1=CC=CC=C1)NC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S.II>>C(C1=CC=CC=C1)N1SC2=NC(=NC=C2C1=O)C1=CC=CC=C1
[O:1]=[C:2]([c:3]1[cH:4][n:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[n:13][c:14]1[SH:15])[NH:16][CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1>>[O:1]=[c:2]1[c:3]2[cH:4][n:5][c:6](-[c:7]3[cH:8][cH:9][cH:10][cH:11][cH:12]3)[n:13][c:14]2[s:15][n:16]1[CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1
O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1S
O=c1c2cnc(-c3ccccc3)nc2sn1Cc1ccccc1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cnc(-c3ccccc3)nc2sn1Cc1ccccc1
[O;D1;H0:1]=[C;H0;D3;+0:2](-[NH;D2;+0:3]-[C:4]-[c:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[O;D1;H0:1]=[c;H0;D3;+0:2]1:[c:6]2:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:2:[s;H0;D2;+0:12]:[n;H0;D3;+0:3]:1-[C:4]-[c:5]
87.6
[{"value": 87.6, "product": "C(C1=CC=CC=C1)N1SC2=NC(=NC=C2C1=O)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 2.0 g (6.22 mmol) of 4-mercapto-2-phenyl-pyrimidine-5-carboxylic acid benzylamide (from Preparation 42) was reacted with 1.74 g (6.8 mmol) of iodine to give 1.74 g of the title compound after crystallization from isopropanol, mp 166°-167° C. Conditions: See reaction.notes.procedure_de...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.c1ccccc1.c1ccccc1
null
null
null
null
O=C(NCc1ccccc1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1Cc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-fa0ff816dc704f9d9450baa6edce85dc
O=C(NCCN1CCOCC1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1CCN1CCOCC1
N1(CCOCC1)CCNC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S.II>>N1(CCOCC1)CCN1SC2=NC(=NC=C2C1=O)C1=CC=CC=C1
[O:1]=[C:2]([c:3]1[cH:4][n:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[n:13][c:14]1[SH:15])[NH:16][CH2:17][CH2:18][N:19]1[CH2:20][CH2:21][O:22][CH2:23][CH2:24]1>>[O:1]=[c:2]1[c:3]2[cH:4][n:5][c:6](-[c:7]3[cH:8][cH:9][cH:10][cH:11][cH:12]3)[n:13][c:14]2[s:15][n:16]1[CH2:17][CH2:18][N:19]1[CH2:20][CH2:21][O:22][CH...
O=C(NCCN1CCOCC1)c1cnc(-c2ccccc2)nc1S
O=c1c2cnc(-c3ccccc3)nc2sn1CCN1CCOCC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cnc(-c3ccccc3)nc2sn1CCN1CCOCC1
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[#7;a:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
60.8
[{"value": 60.8, "product": "N1(CCOCC1)CCN1SC2=NC(=NC=C2C1=O)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 2.0 g (5.81 mmol) of 4-mercapto-2-phenyl-pyrimidine-5-carboxylic acid (2-morpholin-4-yl-ethyl)-amide were treated with 1.47 g (5.81 mmol) of iodine to give 1.21 g of the title compound after recrystallization from isopropanol, mp 163°-165° C. Conditions: See reaction.notes.procedure_d...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.c1ccccc1.C1COCC[NH]1
null
null
null
null
O=C(NCCN1CCOCC1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1CCN1CCOCC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-156358fb63ab4966938ac93b299a8521
O=C(NCCc1ccccc1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1CCc1ccccc1
C(CC1=CC=CC=C1)NC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S.II>>C(CC1=CC=CC=C1)N1SC2=NC(=NC=C2C1=O)C1=CC=CC=C1
[O:1]=[C:2]([c:3]1[cH:4][n:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[n:13][c:14]1[SH:15])[NH:16][CH2:17][CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23][cH:24]1>>[O:1]=[c:2]1[c:3]2[cH:4][n:5][c:6](-[c:7]3[cH:8][cH:9][cH:10][cH:11][cH:12]3)[n:13][c:14]2[s:15][n:16]1[CH2:17][CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23]...
O=C(NCCc1ccccc1)c1cnc(-c2ccccc2)nc1S
O=c1c2cnc(-c3ccccc3)nc2sn1CCc1ccccc1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cnc(-c3ccccc3)nc2sn1CCc1ccccc1
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[#7;a:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
71.5
[{"value": 71.5, "product": "C(CC1=CC=CC=C1)N1SC2=NC(=NC=C2C1=O)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 2.0 g (5.96 mmol) of 4-mercapto-2-phenyl-pyrimidine-5-carboxylic acid phenethyl-amide were treated with 1.66 g (6.56 mmol) of iodine to give 1.42 g of the title compound after recrystallization from isopropanol, mp 144°-147° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.c1ccccc1.c1ccccc1
null
null
null
null
O=C(NCCc1ccccc1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1CCc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9ccc055e75654930ad54bd09e669b039
O=C(NCc1ccccn1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1Cc1ccccn1
N1=C(C=CC=C1)CNC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S.II>>C1(=CC=CC=C1)C1=NC=C2C(=N1)SN(C2=O)CC2=NC=CC=C2
[O:1]=[C:2]([c:3]1[cH:4][n:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[n:13][c:14]1[SH:15])[NH:16][CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][n:23]1>>[O:1]=[c:2]1[c:3]2[cH:4][n:5][c:6](-[c:7]3[cH:8][cH:9][cH:10][cH:11][cH:12]3)[n:13][c:14]2[s:15][n:16]1[CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][n:23]1
O=C(NCc1ccccn1)c1cnc(-c2ccccc2)nc1S
O=c1c2cnc(-c3ccccc3)nc2sn1Cc1ccccn1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cnc(-c3ccccc3)nc2sn1Cc1ccccn1
[#7;a:1]:[c:2]-[C:3]-[NH;D2;+0:4]-[C;H0;D3;+0:5](=[O;D1;H0:6])-[c:7]1:[c:8]:[#7;a:9]:[c:10]:[#7;a:11]:[c:12]:1-[SH;D1;+0:13]>>[#7;a:1]:[c:2]-[C:3]-[n;H0;D3;+0:4]1:[s;H0;D2;+0:13]:[c:12]2:[#7;a:11]:[c:10]:[#7;a:9]:[c:8]:[c:7]:2:[c;H0;D3;+0:5]:1=[O;D1;H0:6]
81.6
[{"value": 81.6, "product": "C1(=CC=CC=C1)C1=NC=C2C(=N1)SN(C2=O)CC2=NC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 2.0 g (6.20 mmol) of 4-mercapto-2-phenyl-pyrimidine-5-carboxylic acid (pyridin-2-ylmethyl)-amide were treated with 1.73 g (6.82 mmol) of iodine to give 1.62 g of the title compound after recrystallization from isopropanol, mp 154°-156° C. Conditions: See reaction.notes.procedure_detai...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.c1ccccc1.c1ccncc1
null
null
null
null
O=C(NCc1ccccn1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1Cc1ccccn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e975da98711c4fb78288d40e04fa9597
O=C(NCCc1ccccn1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1CCc1ccccn1
N1=C(C=CC=C1)CCNC(=O)C=1C(=NC(=NC1)C1=CC=CC=C1)S.II>>C1(=CC=CC=C1)C1=NC=C2C(=N1)SN(C2=O)CCC2=NC=CC=C2
[O:1]=[C:2]([c:3]1[cH:4][n:5][c:6](-[c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12]2)[n:13][c:14]1[SH:15])[NH:16][CH2:17][CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23][n:24]1>>[O:1]=[c:2]1[c:3]2[cH:4][n:5][c:6](-[c:7]3[cH:8][cH:9][cH:10][cH:11][cH:12]3)[n:13][c:14]2[s:15][n:16]1[CH2:17][CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23][...
O=C(NCCc1ccccn1)c1cnc(-c2ccccc2)nc1S
O=c1c2cnc(-c3ccccc3)nc2sn1CCc1ccccn1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cnc(-c3ccccc3)nc2sn1CCc1ccccn1
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[#7;a:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
91.3
[{"value": 91.3, "product": "C1(=CC=CC=C1)C1=NC=C2C(=N1)SN(C2=O)CCC2=NC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 14.0 g (41.6 mmol) of 4-mercapto-2-phenyl-pyrimidine-5-carboxylic acid (2-pyridin-2-yl-ethyl)-amide were treated with 10.6 g (41.7 mmol) of iodine to give 12.7 g of the title compound after recrystallization from ethanol, mp 132°-133° C. Conditions: See reaction.notes.procedure_detail...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.c1ccccc1.c1ccncc1
null
null
null
null
O=C(NCCc1ccccn1)c1cnc(-c2ccccc2)nc1S>>O=c1c2cnc(-c3ccccc3)nc2sn1CCc1ccccn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5f6858b110b847e7ba5291b91729d48c
O=C(NCCc1ccccn1)c1cnc(N2CCCCC2)nc1S>>O=c1c2cnc(N3CCCCC3)nc2sn1CCc1ccccn1
N1=C(C=CC=C1)CCNC(=O)C=1C(=NC(=NC1)N1CCCCC1)S.II>>N1(CCCCC1)C1=NC=C2C(=N1)SN(C2=O)CCC2=NC=CC=C2
[O:1]=[C:2]([c:3]1[cH:4][n:5][c:6]([N:7]2[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)[n:13][c:14]1[SH:15])[NH:16][CH2:17][CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23][n:24]1>>[O:1]=[c:2]1[c:3]2[cH:4][n:5][c:6]([N:7]3[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]3)[n:13][c:14]2[s:15][n:16]1[CH2:17][CH2:18][c:19]1[cH:20][cH:21][cH:22]...
O=C(NCCc1ccccn1)c1cnc(N2CCCCC2)nc1S
O=c1c2cnc(N3CCCCC3)nc2sn1CCc1ccccn1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cnc(N3CCCCC3)nc2sn1CCc1ccccn1
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[#7;a:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
65.2
[{"value": 65.2, "product": "N1(CCCCC1)C1=NC=C2C(=N1)SN(C2=O)CCC2=NC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 33.0 g (96.2 mmol) of 4-mercapto-2-piperidin-1-yl-pyrimidine-5-carboxylic acid (2-pyridin-2-yl-ethyl)-amide were treated with 24.4 g (96.1 mmol) of iodine to give 21.4 g of the title compound after recrystallization from aqueous ethanol, mp 109°-110° C. Conditions: See reaction.notes....
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.C1CC[NH]CC1.c1ccncc1
null
null
null
null
O=C(NCCc1ccccn1)c1cnc(N2CCCCC2)nc1S>>O=c1c2cnc(N3CCCCC3)nc2sn1CCc1ccccn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a80f1938cee54d1f95b65dadd5c69df2
NC(=O)c1cnc(N2CCCCC2)nc1S>>O=c1[nH]sc2nc(N3CCCCC3)ncc12
SC1=NC(=NC=C1C(=O)N)N1CCCCC1.II>>N1(CCCCC1)C1=NC=C2C(=N1)SNC2=O
[O:1]=[C:2]([NH2:3])[c:16]1[c:5]([SH:4])[n:6][c:7]([N:8]2[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]2)[n:14][cH:15]1>>[O:1]=[c:2]1[nH:3][s:4][c:5]2[n:6][c:7]([N:8]3[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]3)[n:14][cH:15][c:16]12
NC(=O)c1cnc(N2CCCCC2)nc1S
O=c1[nH]sc2nc(N3CCCCC3)ncc12
null
null
null
Aromatic Heterocycle Formation
OtherReaction
2b243efd5a58cc7d731ba0d6fa9ecf63de0734418474b3dbffe96158346ff9ac
6b0db660e0291978d674b73a7c89887755b1df41fe1fdc91387cf4ba3ba27df4
O=c1[nH]sc2nc(N3CCCCC3)ncc12
[NH2;D1;+0:1]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[c:4]1:[c:5]:[#7;a:6]:[c:7]:[#7;a:8]:[c:9]:1-[SH;D1;+0:10]>>[O;D1;H0:3]=[c;H0;D3;+0:2]1:[nH;D2;+0:1]:[s;H0;D2;+0:10]:[c:9]2:[#7;a:8]:[c:7]:[#7;a:6]:[c:5]:[c:4]:2:1
69.6
[{"value": 69.6, "product": "N1(CCCCC1)C1=NC=C2C(=N1)SNC2=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 20.8 g (87.4 mmol) of 4-mercapto-2-piperidin-1-yl-pyrimidine-5-carboxylic acid amide were treated with 22.2 g (87.4 mmol) of iodine to give 14.37 g of the title compound after recrystallization from dimethylformamide, mp 268°-269° C. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.C1CC[NH]CC1
null
null
null
null
NC(=O)c1cnc(N2CCCCC2)nc1S>>O=c1[nH]sc2nc(N3CCCCC3)ncc12
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-94a6104e52474749a6d636e419fc633b
O=C(NCCN1CCCCC1)c1cnc(N2CCOCC2)nc1S>>O=c1c2cnc(N3CCOCC3)nc2sn1CCN1CCCCC1
N1(CCCCC1)CCNC(=O)C=1C(=NC(=NC1)N1CCOCC1)S.II>>N1(CCOCC1)C1=NC=C2C(=N1)SN(C2=O)CCN2CCCCC2
[O:1]=[C:2]([c:3]1[cH:4][n:5][c:6]([N:7]2[CH2:8][CH2:9][O:10][CH2:11][CH2:12]2)[n:13][c:14]1[SH:15])[NH:16][CH2:17][CH2:18][N:19]1[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24]1>>[O:1]=[c:2]1[c:3]2[cH:4][n:5][c:6]([N:7]3[CH2:8][CH2:9][O:10][CH2:11][CH2:12]3)[n:13][c:14]2[s:15][n:16]1[CH2:17][CH2:18][N:19]1[CH2:20][CH2:21][CH...
O=C(NCCN1CCCCC1)c1cnc(N2CCOCC2)nc1S
O=c1c2cnc(N3CCOCC3)nc2sn1CCN1CCCCC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cnc(N3CCOCC3)nc2sn1CCN1CCCCC1
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[#7;a:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
50.3
[{"value": 50.3, "product": "N1(CCOCC1)C1=NC=C2C(=N1)SN(C2=O)CCN2CCCCC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 5.2 g (14.8 mmol) of 4-mercapto-2-morpholin-4-yl-pyrimidine-5-carboxylic acid (2-piperidin-1-yl-ethyl)-amide were treated with 3.81 g (15.0 mmol) of iodine to give 2.6 g of the title compound after recrystallization from aqueous isopropanol, mp 98°-100° C. Conditions: See reaction.not...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.C1COCC[NH]1.C1CC[NH]CC1
null
null
null
null
O=C(NCCN1CCCCC1)c1cnc(N2CCOCC2)nc1S>>O=c1c2cnc(N3CCOCC3)nc2sn1CCN1CCCCC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-69d151f088ba4ac0ba3a99cb32f5d727
CN(C)c1ncc(C(=O)NCCc2ccccn2)c(S)n1>>CN(C)c1ncc2c(=O)n(CCc3ccccn3)sc2n1
N1=C(C=CC=C1)CCNC(=O)C=1C(=NC(=NC1)N(C)C)S.II>>CN(C1=NC=C2C(=N1)SN(C2=O)CCC2=NC=CC=C2)C
[CH3:1][N:2]([CH3:3])[c:4]1[n:5][cH:6][c:7]([C:8](=[O:9])[NH:10][CH2:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][n:18]2)[c:20]([SH:19])[n:21]1>>[CH3:1][N:2]([CH3:3])[c:4]1[n:5][cH:6][c:7]2[c:8](=[O:9])[n:10]([CH2:11][CH2:12][c:13]3[cH:14][cH:15][cH:16][cH:17][n:18]3)[s:19][c:20]2[n:21]1
CN(C)c1ncc(C(=O)NCCc2ccccn2)c(S)n1
CN(C)c1ncc2c(=O)n(CCc3ccccn3)sc2n1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cncnc2sn1CCc1ccccn1
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[#7;a:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
56.3
[{"value": 56.3, "product": "CN(C1=NC=C2C(=N1)SN(C2=O)CCC2=NC=CC=C2)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 7.5 g (24.8 mmol) of 2-dimethylamino-4-mercapto-pyrimidine-5-carboxylic acid (2-pyridin-2-yl-ethyl)-amide were treated with 6.4 g (25.2 mmol) of iodine to give 4.21 g of the title compound after recrystallization from isopropanol, mp 134°-136° C. Conditions: See reaction.notes.procedu...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.c1ccncc1
null
null
null
null
CN(C)c1ncc(C(=O)NCCc2ccccn2)c(S)n1>>CN(C)c1ncc2c(=O)n(CCc3ccccn3)sc2n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-02fbceb3836e48fcbd825773c2f9dfe9
CN(C)c1ncc(C(=O)NCCN2CCCCC2)c(S)n1>>CN(C)c1ncc2c(=O)n(CCN3CCCCC3)sc2n1
N1(CCCCC1)CCNC(=O)C=1C(=NC(=NC1)N(C)C)S.II>>CN(C1=NC=C2C(=N1)SN(C2=O)CCN2CCCCC2)C
[CH3:1][N:2]([CH3:3])[c:4]1[n:5][cH:6][c:7]([C:8](=[O:9])[NH:10][CH2:11][CH2:12][N:13]2[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18]2)[c:20]([SH:19])[n:21]1>>[CH3:1][N:2]([CH3:3])[c:4]1[n:5][cH:6][c:7]2[c:8](=[O:9])[n:10]([CH2:11][CH2:12][N:13]3[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18]3)[s:19][c:20]2[n:21]1
CN(C)c1ncc(C(=O)NCCN2CCCCC2)c(S)n1
CN(C)c1ncc2c(=O)n(CCN3CCCCC3)sc2n1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
84d493baceb442fb301ce0e11443d8e4936de615e1a03601e93a225a211a6c68
8f50334308725dd70cedd05b954818305340e80580bc2a806e37bb42f552bc62
O=c1c2cncnc2sn1CCN1CCCCC1
[C:1]-[C:2]-[NH;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c:6]1:[c:7]:[#7;a:8]:[c:9]:[#7;a:10]:[c:11]:1-[SH;D1;+0:12]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[s;H0;D2;+0:12]:[c:11]2:[#7;a:10]:[c:9]:[#7;a:8]:[c:7]:[c:6]:2:[c;H0;D3;+0:4]:1=[O;D1;H0:5]
85.9
[{"value": 85.9, "product": "CN(C1=NC=C2C(=N1)SN(C2=O)CCN2CCCCC2)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example 20, 6.2 g (20.1 mmol) of 2-dimethylamino-4-mercapto-pyrimidine-5-carboxylic acid (2-piperidin-1-yl-ethyl)-amide were treated with 5.08 g (20.0 mmol) of iodine to give 5.31 g of the title compound after recrystallization from ethyl acetate, mp 128°-129° C. Conditions: See reaction.notes.pr...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Aromatic thiol
null
c1cncnc1
c1ncc2cnsc2n1
c1ncc2cnsc2n1.C1CC[NH]CC1
null
null
null
null
CN(C)c1ncc(C(=O)NCCN2CCCCC2)c(S)n1>>CN(C)c1ncc2c(=O)n(CCN3CCCCC3)sc2n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0a13f316069a49f782b0a73c4007b4d6
CC(C)=NO.COC(=O)C12CCCN1CCC2>>Cc1cc(C23CCCN2CCC3)on1
COC(=O)C12CCCN2CCC1.CC(C)=NO.C(CCC)[Li]>>CC1=NOC(=C1)C12CCCN2CCC1
[CH3:1][C:2]([CH3:3])=[N:14][OH:13].CO[C:4](=O)[C:5]12[CH2:6][CH2:7][CH2:8][N:9]1[CH2:10][CH2:11][CH2:12]2>>[CH3:1][c:2]1[cH:3][c:4]([C:5]23[CH2:6][CH2:7][CH2:8][N:9]2[CH2:10][CH2:11][CH2:12]3)[o:13][n:14]1
CC(C)=NO.COC(=O)C12CCCN1CCC2
Cc1cc(C23CCCN2CCC3)on1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
165c42ecc4e9a86073de2acc4f780dc1e165e79d7d4cbb91db7ccb9ad870fea7
b8f4c4009b37b1a89bb4a410e1a9199087d89cbf0a469ca338bf9434c4096abc
c1cc(C23CCCN2CCC3)on1
C-O-[C;H0;D3;+0:1](=O)-[C:2](-[C:3])(-[C:4])-[#7:5](-[C:6])-[C:7].[C;D1;H3:8]-[C;H0;D3;+0:9](-[CH3;D1;+0:10])=[N;H0;D2;+0:11]-[OH;D1;+0:12]>>[C:6]-[#7:5](-[C:7])-[C:2](-[c;H0;D3;+0:1]1:[cH;D2;+0:10]:[c;H0;D3;+0:9](-[C;D1;H3:8]):[n;H0;D2;+0:11]:[o;H0;D2;+0:12]:1)(-[C:3])-[C:4]
11.2
[{"value": 11.0, "product": "CC1=NOC(=C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 11.2, "product": "CC1=NOC(=C1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
8-(Methoxycarbonyl)-hexahydro-1H-pyrrolizine (from step 1d, 1.56 g, 9.22 mmol), acetone oxime (1.45 g, 19.8 mmol) and n-butyllithium (2.5M in hexane, 16 mL, 39.6 mmol) were combined in a similar fashion as that outlined by J. Saunders et at., J. Med. Chem. 1990, 33: 1128. The crude material was chromatographed (silica ...
10.6084/m9.figshare.5104873.v1
null
Ester.Oxime
null
null
c1cnoc1
c1cnoc1.C1CC2CCCN2C1
HO-
null
null
null
CC(C)=NO.COC(=O)C12CCCN1CCC2>>Cc1cc(C23CCCN2CCC3)on1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c8ec9bcee30b4b59a1991ab13c706c61
Cl>>Cl
Cl.CC1=NOC(=C1)C12CCCN2CCC1>>Cl.CC1=NOC(=C1)C12CCCN2CCC1
[ClH:15]>>[ClH:15]
Cl
Cl
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
0
CELSIUS
null
null
7a-(3-methyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (from step 1e, 189 mg, 0.98 mmol) was immersed in Et2O (7 mL) and cooled to 0° C. A solution of Et2O saturated with HCl (g) was added to the reaction vessel dropwise with stirring. The solvent was carefully removed and the remaining white solid triturated with Et2O (2...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
CCOCC
0
null
Cl>CCOCC>Cl
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4a0b85df694b48eb9e5baebab0e7dade
c1cncc(C23CCCN2CCC3)c1>>c1cncc(C23CCCN2CCC3)c1
N1=CC(=CC=C1)C12CCCN2CCC1.CCOCC.Cl>>Cl.N1=CC(=CC=C1)C12CCCN2CCC1
[cH:2]1[cH:3][n:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[cH:15]1>>[cH:2]1[cH:3][n:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[cH:15]1
c1cncc(C23CCCN2CCC3)c1
c1cncc(C23CCCN2CCC3)c1
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
81
[{"value": 81.0, "product": "Cl.N1=CC(=CC=C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
7a-(3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 3a, 125 mg, 0.66 mmol) was dissolved in CH2Cl2 (15 mL) and Et2O saturated with HCl (g) was added dropwise. The solvent was removed, and the remaining solid was triturated with CH2Cl2 (2×) to afford a hygroscopic yellow solid (140 mg, 81%). MS (CI/NH3) m/e: 189 (M+H)+...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
C(Cl)Cl
null
null
c1cncc(C23CCCN2CCC3)c1>C(Cl)Cl>c1cncc(C23CCCN2CCC3)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-56ddd89618f84964b94d7784a2774ae5
Brc1cnc2ccccc2c1.C1CC2=[N+](C1)CCC2>>c1ccc2ncc(C34CCCN3CCC4)cc2c1
Cl.[Li]CCCC.BrC=1C=NC2=CC=CC=C2C1.Cl(=O)(=O)(=O)[O-].C1CC[N+]=2CCCC12>>N1=CC(=CC2=CC=CC=C12)C12CCCN2CCC1
Br[c:7]1[cH:6][n:5][c:4]2[cH:3][cH:2][cH:1][cH:18][c:17]2[cH:16]1.[C:8]12=[N+:12]([CH2:11][CH2:10][CH2:9]1)[CH2:13][CH2:14][CH2:15]2>>[cH:1]1[cH:2][cH:3][c:4]2[n:5][cH:6][c:7]([C:8]34[CH2:9][CH2:10][CH2:11][N:12]3[CH2:13][CH2:14][CH2:15]4)[cH:16][c:17]2[cH:18]1
Brc1cnc2ccccc2c1.C1CC2=[N+](C1)CCC2
c1ccc2ncc(C34CCCN3CCC4)cc2c1
null
null
C1CCOC1.CCOC(=O)C
Functional Group Interconversion
OtherReaction
d081eb00c0c32ed930f1ba0aa9086d7aa7ea50889798160c9d43b81f9c26861b
773dbb8365a8bceadef31887b9f43d5f4f5443038ea5ede92ac6bcd66c5d17b4
c1ccc2ncc(C34CCCN3CCC4)cc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1.[C:7]1-[C:8]-[N+;H0;D3:9]2=[C;H0;D3;+0:10](-[C:11]-[C:12]-[C:13]-2)-[C:14]-1>>[#7;a:5]1:[c:4]:[c:3]:[c:2]:[c;H0;D3;+0:1](-[C;H0;D4;+0:10]23-[C:11]-[C:12]-[C:13]-[N;H0;D3;+0:9]-2-[C:8]-[C:7]-[C:14]-3):[c:6]:1
48.5
[{"value": 46.0, "product": "N1=CC(=CC2=CC=CC=C12)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 48.5, "product": "N1=CC(=CC2=CC=CC=C12)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-100
CELSIUS
2
HOUR
A solution of 2.5M nBuLi (1.2 mL, 2.8 mmol) in hexanes was added to 3-bromoquinoline (386 μL, 2.8 mmol) in THF (10 mL) at -100° C. followed immediately by 1,2,3,5,6,7-hexahydropyrrolizinium perchlorate (200 mg, 0.9 mmol). The reaction mixture was allowed to stir for 2 hours at -100° C. and then 2N HCl was added at 0° C...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Tertiary amine
c1ccc2ncccc2c1.C1CC2=[N+](C1)CCC2
c1ccc2ncccc2c1.C1CC2CCCN2C1
c1ccc2ncccc2c1.C1CC2CCCN2C1
Br-
C1CCOC1.CCOC(=O)C
-100
2
Brc1cnc2ccccc2c1.C1CC2=[N+](C1)CCC2>C1CCOC1.CCOC(=O)C>c1ccc2ncc(C34CCCN3CCC4)cc2c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a738c3035f24486b85c6366c76778e5e
Clc1ccc(C23CCCN2CCC3)cn1>>Clc1ccc(C23CCCN2CCC3)cn1
Cl.ClC1=CC=C(C=N1)C12CCCN2CCC1>>Cl.ClC1=CC=C(C=N1)C12CCCN2CCC1
[Cl:2][c:3]1[cH:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[cH:15][n:16]1>>[Cl:2][c:3]1[cH:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[cH:15][n:16]1
Clc1ccc(C23CCCN2CCC3)cn1
Clc1ccc(C23CCCN2CCC3)cn1
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
155.2
[{"value": 78.0, "product": "Cl.ClC1=CC=C(C=N1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 155.2, "product": "Cl.ClC1=CC=C(C=N1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7a-(6-Chloro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 5a, 210 mg, 0.94 mmol) was dissolved in Et2O (8 mL), and Et2O saturated with HCl (g) was added at ambient temperature. Solvent was then removed, and the remaining solid was recrystallized from MeOH/Et2O to afford short white needles (189 mg, 78%). mp 141°-14...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
CCOCC
null
null
Clc1ccc(C23CCCN2CCC3)cn1>CCOCC>Clc1ccc(C23CCCN2CCC3)cn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5d856ea1f5d4426aaad2bca65084aa0a
Fc1ncccc1C12CCCN1CCC2>>Fc1ncccc1C12CCCN1CCC2
Cl.FC1=NC=CC=C1C12CCCN2CCC1>>Cl.FC1=NC=CC=C1C12CCCN2CCC1
[F:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[C:9]12[CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][CH2:16]2>>[F:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[C:9]12[CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][CH2:16]2
Fc1ncccc1C12CCCN1CCC2
Fc1ncccc1C12CCCN1CCC2
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
77
[{"value": 77.0, "product": "Cl.FC1=NC=CC=C1C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
7a-(2-fluoro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 6a, 59 mg, 0.3 mmol) was dissolved in Et2O (8 mL), and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was recrystallized from MeOH/Et2O to afford a white solid (54 mg, 77%). mp 185°-186° C. MS (CI/NH3) m/e: 207 (M+H)+. 1H...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
CCOCC
null
null
Fc1ncccc1C12CCCN1CCC2>CCOCC>Fc1ncccc1C12CCCN1CCC2
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-092e97d5277f41ea9797e8d42117af0e
Clc1ncccc1C12CCCN1CCC2>>Clc1ncccc1C12CCCN1CCC2
ClC1=NC=CC=C1C12CCCN2CCC1.Cl>>Cl.ClC1=NC=CC=C1C12CCCN2CCC1
[Cl:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[C:9]12[CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][CH2:16]2>>[Cl:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[C:9]12[CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][CH2:16]2
Clc1ncccc1C12CCCN1CCC2
Clc1ncccc1C12CCCN1CCC2
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
null
[]
null
null
null
null
7a-(2-Chloro-3-pyridinyl)-hexahydro-1H-pyrrolizine (21 mg, 0.1 mmol) was dissolved in Et2O (6 mL), and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated (3×) with Et2O to afford a yellow solid (26 mg, quant). mp 186°-188° C. MS (CI/NH3) m/e: 223 (M+H)+. 1H NMR D2O, 300 M...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
CCOCC
null
null
Clc1ncccc1C12CCCN1CCC2>CCOCC>Clc1ncccc1C12CCCN1CCC2
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5e0688aadb234b04b09dab3cc2fb6604
C1CC2=[N+](C1)CCC2.Clc1cc(I)cnc1Cl>>Clc1cc(C23CCCN2CCC3)cnc1Cl
Cl.[Li]C(C)(C)C.ClC1=NC=C(C=C1Cl)I.Cl(=O)(=O)(=O)[O-].C1CC[N+]=2CCCC12>>ClC=1C=C(C=NC1Cl)C12CCCN2CCC1
[C:5]12=[N+:9]([CH2:8][CH2:7][CH2:6]1)[CH2:10][CH2:11][CH2:12]2.I[c:4]1[cH:3][c:2]([Cl:1])[c:15]([Cl:16])[n:14][cH:13]1>>[Cl:1][c:2]1[cH:3][c:4]([C:5]23[CH2:6][CH2:7][CH2:8][N:9]2[CH2:10][CH2:11][CH2:12]3)[cH:13][n:14][c:15]1[Cl:16]
C1CC2=[N+](C1)CCC2.Clc1cc(I)cnc1Cl
Clc1cc(C23CCCN2CCC3)cnc1Cl
null
null
CCCCC.CCOCC
Functional Group Interconversion
OtherReaction
6e757ff9396a07e923211312afac1c080dd23eff3444ff9c846ed5fe9d4243b6
773dbb8365a8bceadef31887b9f43d5f4f5443038ea5ede92ac6bcd66c5d17b4
c1cncc(C23CCCN2CCC3)c1
I-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1.[C:7]1-[C:8]-[C:9]-[C;H0;D3;+0:10]2=[N+;H0;D3:11]-1-[C:12]-[C:13]-[C:14]-2>>[#7;a:3]1:[c:2]:[c;H0;D3;+0:1](-[C;H0;D4;+0:10]23-[C:9]-[C:8]-[C:7]-[N;H0;D3;+0:11]-2-[C:12]-[C:13]-[C:14]-3):[c:6]:[c:5]:[c:4]:1
54.3
[{"value": 54.0, "product": "ClC=1C=C(C=NC1Cl)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 54.3, "product": "ClC=1C=C(C=NC1Cl)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-20
CELSIUS
2
MINUTE
A solution of 1.7M tBuLi (4.7 mL, 8.0 mmol) in pentane was added to 2,3-dichloro-5-iodopyridine (from step 8a, 1.0 g, 3.65 mmol) in Et2O (15 mL) precooled to -100° C. After stirring for 2 minutes, 1,2,3,5,6,7-hexahydropyrrolizinium perchlorate (1.5 g, 7.3 mmol) was added, and the reaction mixture was allowed to stir fo...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Tertiary amine
C1CC2=[N+](C1)CCC2.c1ccncc1
c1ccncc1.C1CC2CCCN2C1
c1ccncc1.C1CC2CCCN2C1
I-
CCCCC.CCOCC
-20
0.033333
C1CC2=[N+](C1)CCC2.Clc1cc(I)cnc1Cl>CCCCC.CCOCC>Clc1cc(C23CCCN2CCC3)cnc1Cl
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ea4bec3ef5714df3ac618bb631d33e9f
Clc1cc(C23CCCN2CCC3)cnc1Cl>>Clc1cc(C23CCCN2CCC3)cnc1Cl
Cl.ClC=1C=C(C=NC1Cl)C12CCCN2CCC1>>Cl.ClC=1C=C(C=NC1Cl)C12CCCN2CCC1
[Cl:2][c:3]1[cH:4][c:5]([C:6]23[CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH2:13]3)[cH:14][n:15][c:16]1[Cl:17]>>[Cl:2][c:3]1[cH:4][c:5]([C:6]23[CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH2:13]3)[cH:14][n:15][c:16]1[Cl:17]
Clc1cc(C23CCCN2CCC3)cnc1Cl
Clc1cc(C23CCCN2CCC3)cnc1Cl
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
151.2
[{"value": 75.0, "product": "Cl.ClC=1C=C(C=NC1Cl)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 151.2, "product": "Cl.ClC=1C=C(C=NC1Cl)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7a-(5,6-dichloro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 8b, 128 mg, 0.50 mmol) was slurried in Et2O (8 mL), and Et2O saturated with HCl (g) added. The solvent was removed, and the solid was recrystallized from MeOH/Et2O to afford a white solid (111 mg, 75%). mp 215°-217° C. MS (CI/NH3) m/e: 257 (M+H)+. 1H NMR...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
CCOCC
null
null
Clc1cc(C23CCCN2CCC3)cnc1Cl>CCOCC>Clc1cc(C23CCCN2CCC3)cnc1Cl
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-00d6327228e6450289cc61943cc4bea5
Brc1cncnc1.C1CC2=[N+](C1)CCC2>>c1ncc(C23CCCN2CCC3)cn1
Cl.[Li]C(C)(C)C.BrC=1C=NC=NC1.Cl(=O)(=O)(=O)[O-].C1CC[N+]=2CCCC12>>N1=CN=CC(=C1)C12CCCN2CCC1
Br[c:4]1[cH:3][n:2][cH:1][n:14][cH:13]1.[C:5]12=[N+:9]([CH2:8][CH2:7][CH2:6]1)[CH2:10][CH2:11][CH2:12]2>>[cH:1]1[n:2][cH:3][c:4]([C:5]23[CH2:6][CH2:7][CH2:8][N:9]2[CH2:10][CH2:11][CH2:12]3)[cH:13][n:14]1
Brc1cncnc1.C1CC2=[N+](C1)CCC2
c1ncc(C23CCCN2CCC3)cn1
null
null
CCCCC.CCOCC.C1CCOC1.CCOCC
Functional Group Interconversion
OtherReaction
c0d44c5278a39501c3cd78edf0b0d4543f902aa8d82206524b4ad2ed2c40732b
773dbb8365a8bceadef31887b9f43d5f4f5443038ea5ede92ac6bcd66c5d17b4
c1ncc(C23CCCN2CCC3)cn1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1.[C:7]1-[C:8]-[C:9]-[C;H0;D3;+0:10]2=[N+;H0;D3:11]-1-[C:12]-[C:13]-[C:14]-2>>[#7;a:3]1:[c:2]:[c;H0;D3;+0:1](-[C;H0;D4;+0:10]23-[C:9]-[C:8]-[C:7]-[N;H0;D3;+0:11]-2-[C:12]-[C:13]-[C:14]-3):[c:6]:[#7;a:5]:[c:4]:1
18
[{"value": 18.0, "product": "N1=CN=CC(=C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 17.6, "product": "N1=CN=CC(=C1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
10
MINUTE
A solution of 1.7M tBuLi (1.6 mL, 2.6 mmol) in pentane was added to 5-bromopyrimidine (190 mg, 1.2 mmol) in Et2O:THF (1:1, 12 mL) at -100° C. After stirring for 10 minutes, 1,2,3,5,6,7-hexahydropyrrolizinium perchlorate (500 mg, 2.4 mmol) was added to the reaction slurry, and stirring was continued for 30 minutes. The ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Tertiary amine
c1cncnc1.C1CC2=[N+](C1)CCC2
c1cncnc1.C1CC2CCCN2C1
c1cncnc1.C1CC2CCCN2C1
Br-
CCCCC.CCOCC.C1CCOC1.CCOCC
0
0.166667
Brc1cncnc1.C1CC2=[N+](C1)CCC2>CCCCC.CCOCC.C1CCOC1.CCOCC>c1ncc(C23CCCN2CCC3)cn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d55b4270d2e84321a49a35cd7ef17438
C1CC2=[N+](C1)CCC2.Fc1cccc(F)n1>>Fc1ccc(C23CCCN2CCC3)c(F)n1
Cl(=O)(=O)(=O)[O-].C1CC[N+]=2CCCC12.[Li]CCCC.C(C)(C)NC(C)C.FC1=NC(=CC=C1)F>>FC1=NC(=CC=C1C12CCCN2CCC1)F
[C:6]12=[N+:10]([CH2:9][CH2:8][CH2:7]1)[CH2:11][CH2:12][CH2:13]2.[F:1][c:2]1[cH:3][cH:4][cH:5][c:14]([F:15])[n:16]1>>[F:1][c:2]1[cH:3][cH:4][c:5]([C:6]23[CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH2:13]3)[c:14]([F:15])[n:16]1
C1CC2=[N+](C1)CCC2.Fc1cccc(F)n1
Fc1ccc(C23CCCN2CCC3)c(F)n1
null
null
C1CCOC1
C-C Coupling
OtherReaction
2744e2374166f7e3b0005d81a2c1df8d47ee0788b4fc7944419feeb27a3619ea
5c03404e5740858973798689d4be0a8ed62608f5043e578ba3cd6de4363e2dbe
c1cncc(C23CCCN2CCC3)c1
[C:1]1-[C:2]-[C:3]-[C;H0;D3;+0:4]2=[N+;H0;D3:5]-1-[C:6]-[C:7]-[C:8]-2.[F;D1;H0:9]-[c:10]1:[#7;a:11]:[c:12]:[c:13]:[c:14]:[cH;D2;+0:15]:1>>[F;D1;H0:9]-[c:10]1:[#7;a:11]:[c:12]:[c:13]:[c:14]:[c;H0;D3;+0:15]:1-[C;H0;D4;+0:4]12-[C:3]-[C:2]-[C:1]-[N;H0;D3;+0:5]-1-[C:6]-[C:7]-[C:8]-2
50.2
[{"value": 50.0, "product": "FC1=NC(=CC=C1C12CCCN2CCC1)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 50.2, "product": "FC1=NC(=CC=C1C12CCCN2CCC1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
10
MINUTE
A solution of 2.5M nBuLi (675 μL, 1.7 mmol) in hexanes was added to diisopropylamine (220 μL, 1.6 mmol) in THF (4.5 mL) at ambient temperature. After 10 minutes of stirring, the reaction mixture was cooled to -78° C., 2,6-difluoropyridine (145 μL, 1.6 mmol) was introduced, and stirring was continued for 1 hour at -78° ...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amine
C1CC2=[N+](C1)CCC2.c1ccncc1
c1ccncc1.C1CC2CCCN2C1
c1ccncc1.C1CC2CCCN2C1
null
C1CCOC1
-78
0.166667
C1CC2=[N+](C1)CCC2.Fc1cccc(F)n1>C1CCOC1>Fc1ccc(C23CCCN2CCC3)c(F)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c055acb214344a499e3a8c789597d987
Fc1ccc(C23CCCN2CCC3)c(F)n1>>Fc1ccc(C23CCCN2CCC3)c(F)n1
Cl.FC1=NC(=CC=C1C12CCCN2CCC1)F>>Cl.FC1=NC(=CC=C1C12CCCN2CCC1)F
[F:2][c:3]1[cH:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[c:15]([F:16])[n:17]1>>[F:2][c:3]1[cH:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[c:15]([F:16])[n:17]1
Fc1ccc(C23CCCN2CCC3)c(F)n1
Fc1ccc(C23CCCN2CCC3)c(F)n1
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
68
[{"value": 68.0, "product": "Cl.FC1=NC(=CC=C1C12CCCN2CCC1)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of Et2O saturated with HCl (g) was added to 7a-(2,6-difluoro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 10a, 174 mg, 0.8 mmol) in Et2O (10 mL). The slurry was filtered, and the filter cake was washed with Et2O to afford a white solid (138 mg, 68%). mp 205°-206° C. MS (CI/NH3) m/e: 225 (M+H)+. 1H NMR D2...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
CCOCC
null
null
Fc1ccc(C23CCCN2CCC3)c(F)n1>CCOCC>Fc1ccc(C23CCCN2CCC3)c(F)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c171067de28743cf9e9bdee6ad6c9574
C1CC2=[N+](C1)CCC2.Clc1cccc(Cl)n1>>Clc1ccc(C23CCCN2CCC3)c(Cl)n1
Cl(=O)(=O)(=O)[O-].C1CC[N+]=2CCCC12.[Li]CCCC.C(C)(C)NC(C)C.Cl.ClC1=NC(=CC=C1)Cl>>ClC1=NC(=CC=C1C12CCCN2CCC1)Cl
[C:6]12=[N+:10]([CH2:9][CH2:8][CH2:7]1)[CH2:11][CH2:12][CH2:13]2.[Cl:1][c:2]1[cH:3][cH:4][cH:5][c:14]([Cl:15])[n:16]1>>[Cl:1][c:2]1[cH:3][cH:4][c:5]([C:6]23[CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH2:13]3)[c:14]([Cl:15])[n:16]1
C1CC2=[N+](C1)CCC2.Clc1cccc(Cl)n1
Clc1ccc(C23CCCN2CCC3)c(Cl)n1
null
null
C1CCOC1.CCOC(=O)C
C-C Coupling
OtherReaction
2744e2374166f7e3b0005d81a2c1df8d47ee0788b4fc7944419feeb27a3619ea
5c03404e5740858973798689d4be0a8ed62608f5043e578ba3cd6de4363e2dbe
c1cncc(C23CCCN2CCC3)c1
[C:1]1-[C:2]-[C:3]-[C;H0;D3;+0:4]2=[N+;H0;D3:5]-1-[C:6]-[C:7]-[C:8]-2.[Cl;D1;H0:9]-[c:10]1:[#7;a:11]:[c:12]:[c:13]:[c:14]:[cH;D2;+0:15]:1>>[Cl;D1;H0:9]-[c:10]1:[#7;a:11]:[c:12]:[c:13]:[c:14]:[c;H0;D3;+0:15]:1-[C;H0;D4;+0:4]12-[C:3]-[C:2]-[C:1]-[N;H0;D3;+0:5]-1-[C:6]-[C:7]-[C:8]-2
17.2
[{"value": 17.0, "product": "ClC1=NC(=CC=C1C12CCCN2CCC1)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 17.2, "product": "ClC1=NC(=CC=C1C12CCCN2CCC1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
10
MINUTE
A solution of 2.5M nBuLi (675 μL, 1.7 mmol) in hexanes was added to diisopropylamine (220 μL, 1.7 mmol) in THF (4.5 mL) at ambient temperature. After 10 minutes of stirring, the reaction mixture was cooled to -78° C., 2,6-dichloropyridine (237 μL, 1.60 mmol) was added neat, and stirring was continued for 1 hour at -78°...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amine
C1CC2=[N+](C1)CCC2.c1ccncc1
c1ccncc1.C1CC2CCCN2C1
c1ccncc1.C1CC2CCCN2C1
null
C1CCOC1.CCOC(=O)C
-78
0.166667
C1CC2=[N+](C1)CCC2.Clc1cccc(Cl)n1>C1CCOC1.CCOC(=O)C>Clc1ccc(C23CCCN2CCC3)c(Cl)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6a4ede5955b04d74b49bc94baae656f9
Clc1ccc(C23CCCN2CCC3)c(Cl)n1>>Clc1ccc(C23CCCN2CCC3)c(Cl)n1
Cl.ClC1=NC(=CC=C1C12CCCN2CCC1)Cl>>Cl.ClC1=NC(=CC=C1C12CCCN2CCC1)Cl
[Cl:2][c:3]1[cH:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[c:15]([Cl:16])[n:17]1>>[Cl:2][c:3]1[cH:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[c:15]([Cl:16])[n:17]1
Clc1ccc(C23CCCN2CCC3)c(Cl)n1
Clc1ccc(C23CCCN2CCC3)c(Cl)n1
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
101
[{"value": 101.0, "product": "Cl.ClC1=NC(=CC=C1C12CCCN2CCC1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7a-(2,6-dichloro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 11a, 62 mg, 0.24 mmol) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated with Et2O to give a white solid (35.6 mg). mp 212°-214° C. 1H NMR D2O, 300 MHz) δ2.02-2.18 (m, 2H), 2.28-...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
CCOCC
null
null
Clc1ccc(C23CCCN2CCC3)c(Cl)n1>CCOCC>Clc1ccc(C23CCCN2CCC3)c(Cl)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c3b0e2987bf6463288457f21739f34ea
O=[N+]([O-])c1ccc(Cl)nc1.[F-]>>O=[N+]([O-])c1ccc(F)nc1
ClC1=NC=C(C=C1)[N+](=O)[O-].[F-].[K+].C(C)#N>>FC1=NC=C(C=C1)[N+](=O)[O-]
Cl[c:7]1[cH:6][cH:5][c:4]([N+:2](=[O:1])[O-:3])[cH:10][n:9]1.[F-:8]>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([F:8])[n:9][cH:10]1
O=[N+]([O-])c1ccc(Cl)nc1.[F-]
O=[N+]([O-])c1ccc(F)nc1
null
[P+](C1=CC=CC=C1)(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.[Br-]
CCOCC
Functional Group Interconversion
OtherReaction
c5ee9801df82c43b4536f3b3bcf4d5fc4f4f88678c4231db54140fcd8ba626c5
4131cd1655d0ec8ecf7e181a36ab37eb3293d734e38ece0acf0e59405d170401
c1ccncc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5].[F-;H0;D0:6]>>[F;H0;D1;+0:6]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
null
null
2-Chloro-5-nitropyridine (100 g, 0.656 mol, Aldrich), KF (84.1 g, 1.448 mol), Ph4PBr (95.3 g, 0.227 mol) and acetonitrile (1.5 L) were combined and heated at reflux until no starting material remained. The volume was reduced to 750 mL, and the mixture was diluted with 2 L of ether, filtered and concentrated. The residu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Aromatic halide
c1ccncc1
c1ccncc1
c1ccncc1
Other
[P+](C1=CC=CC=C1)(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.[Br-].CCOCC
null
null
O=[N+]([O-])c1ccc(Cl)nc1.[F-]>[P+](C1=CC=CC=C1)(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.[Br-].CCOCC>O=[N+]([O-])c1ccc(F)nc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d3051c784ee74eefb4384c960765bcf2
C1CC2=[N+](C1)CCC2.Fc1ccc(I)cn1>>Fc1ccc(C23CCCN2CCC3)cn1
FC1=NC=C(C=C1)I.[Li]C(C)(C)C.Cl(=O)(=O)(=O)[O-].C1CC[N+]=2CCCC12>>FC1=CC=C(C=N1)C12CCCN2CCC1
[C:6]12=[N+:10]([CH2:9][CH2:8][CH2:7]1)[CH2:11][CH2:12][CH2:13]2.I[c:5]1[cH:4][cH:3][c:2]([F:1])[n:15][cH:14]1>>[F:1][c:2]1[cH:3][cH:4][c:5]([C:6]23[CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH2:13]3)[cH:14][n:15]1
C1CC2=[N+](C1)CCC2.Fc1ccc(I)cn1
Fc1ccc(C23CCCN2CCC3)cn1
null
null
CCCCC.CCOCC
Functional Group Interconversion
OtherReaction
6e757ff9396a07e923211312afac1c080dd23eff3444ff9c846ed5fe9d4243b6
773dbb8365a8bceadef31887b9f43d5f4f5443038ea5ede92ac6bcd66c5d17b4
c1cncc(C23CCCN2CCC3)c1
I-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1.[C:7]1-[C:8]-[C:9]-[C;H0;D3;+0:10]2=[N+;H0;D3:11]-1-[C:12]-[C:13]-[C:14]-2>>[#7;a:3]1:[c:2]:[c;H0;D3;+0:1](-[C;H0;D4;+0:10]23-[C:9]-[C:8]-[C:7]-[N;H0;D3;+0:11]-2-[C:12]-[C:13]-[C:14]-3):[c:6]:[c:5]:[c:4]:1
40.4
[{"value": 40.0, "product": "FC1=CC=C(C=N1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 40.4, "product": "FC1=CC=C(C=N1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
2
MINUTE
2-Fluoro-5-iodopyridine (200 μL, 0.90 mmol) was dissolved in Et2O and cooled to -78° C. A solution of 2.5M t-BuLi (1.2 mL, 1.98 mmol) in pentane was added, and the reaction was stirred for 2 minutes. 1,2,3,5,6,7-hexahydropyrrolizinium perchlorate (375 mg, 1.80 mmol) was added, and the reaction mixture was allowed to st...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Tertiary amine
C1CC2=[N+](C1)CCC2.c1ccncc1
c1ccncc1.C1CC2CCCN2C1
c1ccncc1.C1CC2CCCN2C1
I-
CCCCC.CCOCC
-78
0.033333
C1CC2=[N+](C1)CCC2.Fc1ccc(I)cn1>CCCCC.CCOCC>Fc1ccc(C23CCCN2CCC3)cn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-b9f158cd252c4dcaaab2ab046391e1e9
Fc1cncc(C23CCCN2CCC3)c1>>Fc1cncc(C23CCCN2CCC3)c1
Cl.FC=1C=C(C=NC1)C12CCCN2CCC1>>Cl.FC=1C=C(C=NC1)C12CCCN2CCC1
[F:2][c:3]1[cH:4][n:5][cH:6][c:7]([C:8]23[CH2:9][CH2:10][CH2:11][N:12]2[CH2:13][CH2:14][CH2:15]3)[cH:16]1>>[F:2][c:3]1[cH:4][n:5][cH:6][c:7]([C:8]23[CH2:9][CH2:10][CH2:11][N:12]2[CH2:13][CH2:14][CH2:15]3)[cH:16]1
Fc1cncc(C23CCCN2CCC3)c1
Fc1cncc(C23CCCN2CCC3)c1
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
69
[{"value": 69.0, "product": "Cl.FC=1C=C(C=NC1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
7a-(5-fluoro-3-pyridinyl)-hexahydro-1H-pyrrolizine (62 mg, 0.24 mmol, from step 12d) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated with to give a white solid (57.1 mg, 69%). mp 168°-169° C. 1H NMR D2O, 300 MHz) 67 2.13-2.50 (m, 6H), 2.58-2....
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
CCOCC
null
null
Fc1cncc(C23CCCN2CCC3)c1>CCOCC>Fc1cncc(C23CCCN2CCC3)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-eafa3d7b107148f580724adaf23e414c
[CH+]1CCN2CCCC12>>C#CC12CCCN1CCC2
Cl(=O)(=O)(=O)[O-].[CH+]1CCN2CCCC12.C(#C)[Mg]Br.[OH-].[Na+]>>C(#C)C12CCCN2CCC1
[CH:3]12[CH2:4][CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][CH+:10]2>>[CH:1]#[C:2][C:3]12[CH2:4][CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][CH2:10]2
[CH+]1CCN2CCCC12
C#CC12CCCN1CCC2
null
null
[Cl-].[Na+].O.O.C1CCOC1
Functional Group Interconversion
OtherReaction
b404c07d8cc44b859c403c8f07b0facb1ff137e72068444aa4bfd36e8160f6a7
c4460923656748296c1ad8c3927d77d5a4d016526df2201ea5f91f81ef0c2060
C1CC2CCCN2C1
[C:1]1-[C:2]-[C:3]-[#7:4]2-[C:5]-[C:6]-[CH+;D2:7]-[CH;D3;+0:8]-1-2>>[C;D1;H1:9]#[C:10]-[C;H0;D4;+0:8]12-[C:1]-[C:2]-[C:3]-[#7:4]-1-[C:5]-[C:6]-[CH2;D2;+0:7]-2
71.3
[{"value": 71.0, "product": "C(#C)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 71.3, "product": "C(#C)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
45
MINUTE
1,2,3,5,6,7-Hexahydropyrrolizinylium perchlorate (1.0 g, 4.8 mmol) was added to a solution of 0.5M ethynylmagnesium bromide (29 mL, 14.3 mmol) in THF at room temperature. The reaction mixture was allowed to stir for 45 minutes, and 15% NaOH solution was added. The slurry was diluted with brine:water (1:1) and extracted...
10.6084/m9.figshare.5104873.v1
null
null
Alkyne
[CH+]1CCN2CCCC12
C1CC2CCCN2C1
C1CC2CCCN2C1
null
[Cl-].[Na+].O.O.C1CCOC1
null
0.75
[CH+]1CCN2CCCC12>[Cl-].[Na+].O.O.C1CCOC1>C#CC12CCCN1CCC2
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8757226fe4fa4085a41ed03eefc15d62
C#CC12CCCN1CCC2.CCC[N+](=O)[O-]>>CCc1cc(C23CCCN2CCC3)on1
[N+](=O)([O-])CCC.C1(=CC=CC=C1)N=C=O.C(#C)C12CCCN2CCC1>>C(C)C1=NOC(=C1)C12CCCN2CCC1
[CH:4]#[C:5][C:6]12[CH2:7][CH2:8][CH2:9][N:10]1[CH2:11][CH2:12][CH2:13]2.O=[N+:15]([CH2:3][CH2:2][CH3:1])[O-:14]>>[CH3:1][CH2:2][c:3]1[cH:4][c:5]([C:6]23[CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH2:13]3)[o:14][n:15]1
C#CC12CCCN1CCC2.CCC[N+](=O)[O-]
CCc1cc(C23CCCN2CCC3)on1
null
null
C1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
85ed1de7d01eb5a1475dc4727791ddb53417125ab3beeb28225b6652ffdb9c73
7108617e87a7921f39c453b93eea7dbd08d46222031ed4533f4e27c039907e0d
c1cc(C23CCCN2CCC3)on1
O=[N+;H0;D3:1](-[O-;H0;D1:2])-[CH2;D2;+0:3]-[C:4]-[C;D1;H3:5].[C:6]-[#7:7](-[C:8])-[C:9](-[C;H0;D2;+0:10]#[CH;D1;+0:11])(-[C:12])-[C:13]>>[C:6]-[#7:7](-[C:8])-[C:9](-[c;H0;D3;+0:10]1:[cH;D2;+0:11]:[c;H0;D3;+0:3](-[C:4]-[C;D1;H3:5]):[n;H0;D2;+0:1]:[o;H0;D2;+0:2]:1)(-[C:12])-[C:13]
50.1
[{"value": 50.0, "product": "C(C)C1=NOC(=C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 50.1, "product": "C(C)C1=NOC(=C1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
Nitropropane (0.475 mL, 5.29 mmol) and phenylisocyanate (1.0 mL, 9.5 mmol) were dissolved in benzene (10 mL) and added to a flask containing 7a-ethynyl-hexahydro-1H-pyrrolizine (358 mg, 2.65 mmol, from step 13a). The solution was stirred at ambient temperature for 1 hour and at reflux for 5 hours. The mixture was coole...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Alkyne
null
null
c1cnoc1
c1cnoc1.C1CC2CCCN2C1
HO-
C1=CC=CC=C1
null
1
C#CC12CCCN1CCC2.CCC[N+](=O)[O-]>C1=CC=CC=C1>CCc1cc(C23CCCN2CCC3)on1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6a17fe06ca0a4559821af5872f757c00
Cl>>Cl
Cl.C(C)C1=NOC(=C1)C12CCCN2CCC1>>Cl.C(C)C1=NOC(=C1)C12CCCN2CCC1
[ClH:16]>>[ClH:16]
Cl
Cl
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
null
null
null
null
7a-(3-ethyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (265 mg, 1.30 mmol, from step 13b) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was recrystallized from methanol/ethanol to afford the title compound as a white solid: mp 139°-140° C.; 1H NMR D2O, 300 MH...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
CCOCC
null
null
Cl>CCOCC>Cl
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-bbc0aabc6c144848bb5aa35cb5124c07
C#CC12CCCN1CCC2.CCCC[N+](=O)[O-]>>CCCc1cc(C23CCCN2CCC3)on1
[N+](=O)([O-])CCCC.C1(=CC=CC=C1)N=C=O.C(#C)C12CCCN2CCC1>>C(CC)C1=NOC(=C1)C12CCCN2CCC1
[CH:5]#[C:6][C:7]12[CH2:8][CH2:9][CH2:10][N:11]1[CH2:12][CH2:13][CH2:14]2.O=[N+:16]([CH2:4][CH2:3][CH2:2][CH3:1])[O-:15]>>[CH3:1][CH2:2][CH2:3][c:4]1[cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[o:15][n:16]1
C#CC12CCCN1CCC2.CCCC[N+](=O)[O-]
CCCc1cc(C23CCCN2CCC3)on1
null
null
C1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
85ed1de7d01eb5a1475dc4727791ddb53417125ab3beeb28225b6652ffdb9c73
7108617e87a7921f39c453b93eea7dbd08d46222031ed4533f4e27c039907e0d
c1cc(C23CCCN2CCC3)on1
O=[N+;H0;D3:1](-[O-;H0;D1:2])-[CH2;D2;+0:3]-[C:4]-[C:5].[C:6]-[#7:7](-[C:8])-[C:9](-[C;H0;D2;+0:10]#[CH;D1;+0:11])(-[C:12])-[C:13]>>[C:6]-[#7:7](-[C:8])-[C:9](-[c;H0;D3;+0:10]1:[cH;D2;+0:11]:[c;H0;D3;+0:3](-[C:4]-[C:5]):[n;H0;D2;+0:1]:[o;H0;D2;+0:2]:1)(-[C:12])-[C:13]
53.4
[{"value": 53.0, "product": "C(CC)C1=NOC(=C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 53.4, "product": "C(CC)C1=NOC(=C1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
Nitrobutane (0.705 mL, 6.66 mmol) and phenylisocyanate (1.50 mL, 13.3 mmol) were dissolved in benzene (13.5 mL) and added to a flask containing 7a-ethynyl-hexahydro-1H-pyrrolizine (450 mg, 3.33 mmol, from step 13a). The solution was stirred at ambient temperature for 1 hour and at reflux for 5 hours. The mixture was co...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Alkyne
null
null
c1cnoc1
c1cnoc1.C1CC2CCCN2C1
HO-
C1=CC=CC=C1
null
1
C#CC12CCCN1CCC2.CCCC[N+](=O)[O-]>C1=CC=CC=C1>CCCc1cc(C23CCCN2CCC3)on1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-402839b675474c22a8bd5c354e9adae4
Cl>>Cl
Cl.C(CC)C1=NOC(=C1)C12CCCN2CCC1>>Cl.C(CC)C1=NOC(=C1)C12CCCN2CCC1
[ClH:17]>>[ClH:17]
Cl
Cl
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
null
null
null
null
7a-(3-propyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (265 mg, 1.30 mmol, from step 14a) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated with Et2O and dried to afford the title compound as a free flowing white powder. mp 97°-98° C. MS (NH3 /CI)...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
CCOCC
null
null
Cl>CCOCC>Cl
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e4c5a915e9a24293aae0af7d3e5b3bcb
C[N+](=O)[O-].O=Cc1ccccc1>>O=[N+]([O-])C=Cc1ccccc1
Cl.C(C1=CC=CC=C1)=O.[N+](=O)([O-])C.[OH-].[Na+]>>C1(=CC=CC=C1)C=C[N+](=O)[O-]
[O:1]=[N+:2]([O-:3])[CH3:4].O=[CH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1>>[O:1]=[N+:2]([O-:3])[CH:4]=[CH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1
C[N+](=O)[O-].O=Cc1ccccc1
O=[N+]([O-])C=Cc1ccccc1
null
null
CO
C-C Coupling
OtherReaction
7ede86d40d3d69f429dde089476c8b7ffa9b74bf3050590255e6323d013c2daf
f736727903c0ad5511d468246b8e380897fd19905174c118ffa4ed4d3651f6ea
c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[#7;+:6](-[O;-;D1;H0:7])=[O;D1;H0:8]>>[O;-;D1;H0:7]-[#7;+:6](=[O;D1;H0:8])-[CH;D2;+0:5]=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]
37
[{"value": 37.0, "product": "C1(=CC=CC=C1)C=C[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 36.7, "product": "C1(=CC=CC=C1)C=C[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-18
CELSIUS
2
HOUR
Benzaldehyde (10.0 g, 94.2 mmol) and nitromethane (5.1 mL, 94.2 mmol) were dissolved in MeOH, the solution was cooled to -18° C., and NaOH (3.9 g, 98.9 mmol) in aqueous solution (80 mL) was added while maintaining the temperature below -10° C. The mixture was stirred at 0° C. for 2 hours, then stored at 5° C. overnight...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Nitro group
Enamine
null
null
c1ccccc1
HO-
CO
-18
2
C[N+](=O)[O-].O=Cc1ccccc1>CO>O=[N+]([O-])C=Cc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d656571e780d4bccad9fd6471b2c4bc3
O=[N+]([O-])C=Cc1ccccc1>>O=[N+]([O-])CCc1ccccc1
Cl.C1(=CC=CC=C1)C=C[N+](=O)[O-].[BH4-].[Na+]>>C1(=CC=CC=C1)CC[N+](=O)[O-]
[O:1]=[N+:2]([O-:3])[CH:4]=[CH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1>>[O:1]=[N+:2]([O-:3])[CH2:4][CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1
O=[N+]([O-])C=Cc1ccccc1
O=[N+]([O-])CCc1ccccc1
null
null
C(Cl)(Cl)Cl.CC(C)O
Reduction
Hydrogenation (double to single)
1897ddb5557a7164dfa80083adb557accafa4233396f9576d5bfde28d2818919
92f8c31381fee05ef128b294b51ee13ebdada3b3789c3c4a7dc0a1d2ea4408c2
c1ccccc1
[O;-;D1;H0:1]-[#7;+:2](=[O;D1;H0:3])-[CH;D2;+0:4]=[CH;D2;+0:5]-[c:6](:[c:7]):[c:8]>>[O;-;D1;H0:1]-[#7;+:2](=[O;D1;H0:3])-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[c:6](:[c:7]):[c:8]
75
[{"value": 75.0, "product": "C1(=CC=CC=C1)CC[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.0, "product": "C1(=CC=CC=C1)CC[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
90
MINUTE
2-Phenylnitroethene (5.12 g, 34.3 mmol, from step 15a) was dissolved in CHCl3 /i-PrOH (410:85 mL) and SiO2 (51.4 g) was added. NaBH4 (5.2 g, 137 mmol) was added in portions, and the mixture was stirred for 90 minutes at room temperature. HCl (0.5N, 100, mL) was added, and the mixture was stirred for 30 minutes. The lay...
10.6084/m9.figshare.5104873.v1
null
Enamine
Nitro group
null
null
c1ccccc1
null
C(Cl)(Cl)Cl.CC(C)O
null
1.5
O=[N+]([O-])C=Cc1ccccc1>C(Cl)(Cl)Cl.CC(C)O>O=[N+]([O-])CCc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-58fe89ee31bc421fa1afea328a51d6a8
C#CC12CCCN1CCC2.O=[N+]([O-])CCc1ccccc1>>c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
C1(=CC=CC=C1)CC[N+](=O)[O-].C1(=CC=CC=C1)N=C=O.C(#C)C12CCCN2CCC1>>C(C1=CC=CC=C1)C1=NOC(=C1)C12CCCN2CCC1
[CH:7]#[C:8][C:9]12[CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][CH2:16]2.O=[N+:18]([CH2:6][CH2:5][c:4]1[cH:3][cH:2][cH:1][cH:20][cH:19]1)[O-:17]>>[cH:1]1[cH:2][cH:3][c:4]([CH2:5][c:6]2[cH:7][c:8]([C:9]34[CH2:10][CH2:11][CH2:12][N:13]3[CH2:14][CH2:15][CH2:16]4)[o:17][n:18]2)[cH:19][cH:20]1
C#CC12CCCN1CCC2.O=[N+]([O-])CCc1ccccc1
c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
null
null
C1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
85ed1de7d01eb5a1475dc4727791ddb53417125ab3beeb28225b6652ffdb9c73
7108617e87a7921f39c453b93eea7dbd08d46222031ed4533f4e27c039907e0d
c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
O=[N+;H0;D3:1](-[O-;H0;D1:2])-[CH2;D2;+0:3]-[C:4]-[c:5].[C:6]-[C:7](-[C;H0;D2;+0:8]#[CH;D1;+0:9])(-[C:10])-[#7:11](-[C:12])-[C:13]>>[C:6]-[C:7](-[c;H0;D3;+0:8]1:[cH;D2;+0:9]:[c;H0;D3;+0:3](-[C:4]-[c:5]):[n;H0;D2;+0:1]:[o;H0;D2;+0:2]:1)(-[C:10])-[#7:11](-[C:12])-[C:13]
52.2
[{"value": 52.0, "product": "C(C1=CC=CC=C1)C1=NOC(=C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 52.2, "product": "C(C1=CC=CC=C1)C1=NOC(=C1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Phenylnitroethane (895 mg, 5.92 mmol, from step 15b) and phenylisocyanate (1.3 mL, 11.8 mmol) were dissolved in benzene (12 mL) and added to a flask containing 7a-ethynyl-hexahydro-1H-pyrrolizine (400 mg, 2.96 mmol, from step 13a). The solution was stirred at reflux for 5 hours, cooled and stirred for 48 hours at roo...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Alkyne
null
null
c1cnoc1
c1ccccc1.c1cnoc1.C1CC2CCCN2C1
HO-
C1=CC=CC=C1
null
null
C#CC12CCCN1CCC2.O=[N+]([O-])CCc1ccccc1>C1=CC=CC=C1>c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-72dde4f2823b4e96864c3d6a03b9a1bd
c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1>>c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
Cl.C(C1=CC=CC=C1)C1=NOC(=C1)C12CCCN2CCC1>>Cl.C(C1=CC=CC=C1)C1=NOC(=C1)C12CCCN2CCC1
[cH:2]1[cH:3][cH:4][c:5]([CH2:6][c:7]2[cH:8][c:9]([C:10]34[CH2:11][CH2:12][CH2:13][N:14]3[CH2:15][CH2:16][CH2:17]4)[o:18][n:19]2)[cH:20][cH:21]1>>[cH:2]1[cH:3][cH:4][c:5]([CH2:6][c:7]2[cH:8][c:9]([C:10]34[CH2:11][CH2:12][CH2:13][N:14]3[CH2:15][CH2:16][CH2:17]4)[o:18][n:19]2)[cH:20][cH:21]1
c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
null
null
CCOCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
null
null
[]
null
null
null
null
7a-(3-Benzyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (407 mg, 1.52 mmol, from step 15c) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was recrystallized from MeOH and dried to afford the title compound as white needles: mp 126°-127° C.; 1H NMR D2O, 300 MHz...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1cnoc1.C1CC2CCCN2C1
null
CCOCC
null
null
c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1>CCOCC>c1ccc(Cc2cc(C34CCCN3CCC4)on2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4279b67233d44b409a5090ce4f747f2e
Brc1cncc(Br)c1.OCc1ccccc1>>Brc1cncc(OCc2ccccc2)c1
[NH4+].[Cl-].C(C1=CC=CC=C1)O.[H-].[Na+].BrC=1C=NC=C(C1)Br>>C(C1=CC=CC=C1)OC=1C=NC=C(C1)Br
Br[c:6]1[cH:5][n:4][cH:3][c:2]([Br:1])[cH:15]1.[OH:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1>>[Br:1][c:2]1[cH:3][n:4][cH:5][c:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[cH:15]1
Brc1cncc(Br)c1.OCc1ccccc1
Brc1cncc(OCc2ccccc2)c1
null
null
CN(C)C=O.O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
ea617b323b892eda23f5ae30e789991ea9692064ef355a16e8ed81c16e743d2b
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1ccc(COc2cccnc2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1.[OH;D1;+0:7]-[C:8]-[c:9]>>[c:9]-[C:8]-[O;H0;D2;+0:7]-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1
72.1
[{"value": 72.0, "product": "C(C1=CC=CC=C1)OC=1C=NC=C(C1)Br", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.1, "product": "C(C1=CC=CC=C1)OC=1C=NC=C(C1)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
Sodium hydride (60% in mineral oil, 40.9 g, 1.0 mol) in DMF (800 mL) was cooled to 0° C., and benzyl alcohol (105 mL, 1.0 mol) was slowly added. After stirring for 1 hour at ambient temperature, 3,5-dibromopyridine (200.4 g, 846 mmol) was added and the mixture allowed to stir for 16 hours. Saturated NH4Cl solution (500...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1ccncc1
c1ccncc1
c1ccncc1.c1ccccc1
HBr
CN(C)C=O.O
null
1
Brc1cncc(Br)c1.OCc1ccccc1>CN(C)C=O.O>Brc1cncc(OCc2ccccc2)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-227b359fc5e7487cb58b11323a1b2724
Brc1cncc(OCc2ccccc2)c1.C1CC2=[N+](C1)CCC2>>c1ccc(COc2cncc(C34CCCN3CCC4)c2)cc1
C(C1=CC=CC=C1)OC=1C=NC=C(C1)Br.[Li]C(C)(C)C.Cl(=O)(=O)(=O)[O-].C1CC[N+]=2CCCC12>>C(C1=CC=CC=C1)OC=1C=NC=C(C1)C12CCCN2CCC1
Br[c:11]1[cH:10][n:9][cH:8][c:7]([O:6][CH2:5][c:4]2[cH:3][cH:2][cH:1][cH:22][cH:21]2)[cH:20]1.[C:12]12=[N+:16]([CH2:15][CH2:14][CH2:13]1)[CH2:17][CH2:18][CH2:19]2>>[cH:1]1[cH:2][cH:3][c:4]([CH2:5][O:6][c:7]2[cH:8][n:9][cH:10][c:11]([C:12]34[CH2:13][CH2:14][CH2:15][N:16]3[CH2:17][CH2:18][CH2:19]4)[cH:20]2)[cH:21][cH:22]...
Brc1cncc(OCc2ccccc2)c1.C1CC2=[N+](C1)CCC2
c1ccc(COc2cncc(C34CCCN3CCC4)c2)cc1
null
null
CCCCC.CCOCC
Functional Group Interconversion
OtherReaction
6e757ff9396a07e923211312afac1c080dd23eff3444ff9c846ed5fe9d4243b6
773dbb8365a8bceadef31887b9f43d5f4f5443038ea5ede92ac6bcd66c5d17b4
c1ccc(COc2cncc(C34CCCN3CCC4)c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1.[C:7]1-[C:8]-[C:9]-[N+;H0;D3:10]2=[C;H0;D3;+0:11]-1-[C:12]-[C:13]-[C:14]-2>>[#7;a:3]1:[c:2]:[c;H0;D3;+0:1](-[C;H0;D4;+0:11]23-[C:7]-[C:8]-[C:9]-[N;H0;D3;+0:10]-2-[C:14]-[C:13]-[C:12]-3):[c:6]:[c:5]:[c:4]:1
22
[{"value": 22.0, "product": "C(C1=CC=CC=C1)OC=1C=NC=C(C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 21.7, "product": "C(C1=CC=CC=C1)OC=1C=NC=C(C1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
10
MINUTE
3-Benzyloxy-5-bromopyridine (1.18 g, 4.47 mmol) was dissolved in Et2O and cooled to -78° C. A solution of 2.5M t-BuLi (5.8 mL, 9.83 mmol) in pentane was added, and the reaction was stirred for 10 minutes. 1,2,3,5,6,7-hexahydropyrrolizinium perchlorate (1.4 g, 6.70 mmol) was added, and the reaction mixture was allowed t...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Tertiary amine
c1ccncc1.C1CC2=[N+](C1)CCC2
c1ccncc1.C1CC2CCCN2C1
c1ccccc1.c1ccncc1.C1CC2CCCN2C1
Br-
CCCCC.CCOCC
-78
0.166667
Brc1cncc(OCc2ccccc2)c1.C1CC2=[N+](C1)CCC2>CCCCC.CCOCC>c1ccc(COc2cncc(C34CCCN3CCC4)c2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-94eabea82a724e06b470656c1d0fc4ec
c1ccc(COc2cncc(C34CCCN3CCC4)c2)cc1>>Oc1cncc(C23CCCN2CCC3)c1
C(C1=CC=CC=C1)OC=1C=NC=C(C1)C12CCCN2CCC1>>OC=1C=NC=C(C1)C12CCCN2CCC1
c1ccc(C[O:1][c:2]2[cH:3][n:4][cH:5][c:6]([C:7]34[CH2:8][CH2:9][CH2:10][N:11]3[CH2:12][CH2:13][CH2:14]4)[cH:15]2)cc1>>[OH:1][c:2]1[cH:3][n:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[cH:15]1
c1ccc(COc2cncc(C34CCCN3CCC4)c2)cc1
Oc1cncc(C23CCCN2CCC3)c1
null
[Pt]
CO
Deprotection
Hydroxyl benzyl deprotection
36869d1fe85185a14d9eb30bf05178c600a9b6eca277ffaf3803578c30e0bf5d
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1cncc(C23CCCN2CCC3)c1
[c:1]:[c:2](-[O;H0;D2;+0:3]-C-c1:c:c:c:c:c:1):[c:4]:[#7;a:5]:[c:6]>>[OH;D1;+0:3]-[c:2](:[c:1]):[c:4]:[#7;a:5]:[c:6]
63.4
[{"value": 63.0, "product": "OC=1C=NC=C(C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 63.4, "product": "OC=1C=NC=C(C1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
7a-(3-Benzyloxy-5-pyridinyl)-hexahydro-1H-pyrrolizine (260 mg, 0.88 mmol, from step 16b) was dissolved in methanol (9 mL), 10% Pt/C (35 mg) was added, and the mixture stirred under 1 arm of H2 for 16 hours. The catalyst was removed, the filtrate was concentrated, and the residue was chromatographed (silica gel; CHCl3 /...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
c1ccccc1
null
c1ccncc1.C1CC2CCCN2C1
Other
[Pt].CO
null
16
c1ccc(COc2cncc(C34CCCN3CCC4)c2)cc1>[Pt].CO>Oc1cncc(C23CCCN2CCC3)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-024cc166a8ad4750aa817d400f40ba7a
Oc1cncc(C23CCCN2CCC3)c1>>Oc1cncc(C23CCCN2CCC3)c1
OC=1C=NC=C(C1)C12CCCN2CCC1.CCOCC.Cl>>Cl.OC=1C=NC=C(C1)C12CCCN2CCC1
[OH:2][c:3]1[cH:4][n:5][cH:6][c:7]([C:8]23[CH2:9][CH2:10][CH2:11][N:12]2[CH2:13][CH2:14][CH2:15]3)[cH:16]1>>[OH:2][c:3]1[cH:4][n:5][cH:6][c:7]([C:8]23[CH2:9][CH2:10][CH2:11][N:12]2[CH2:13][CH2:14][CH2:15]3)[cH:16]1
Oc1cncc(C23CCCN2CCC3)c1
Oc1cncc(C23CCCN2CCC3)c1
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cncc(C23CCCN2CCC3)c1
null
91
[{"value": 91.0, "product": "Cl.OC=1C=NC=C(C1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
7a-(3-Hydroxy-5-pyridinyl)-hexahydro-1H-pyrrolizine (150 mg, 0.56 mmol, from step 16c) was dissolved in methylene chloride, and Et2O saturated with HCl (g) was added. The solvent was removed, and the solid was dried to afford the title compound as a white powder (114 mg, 91%): mp 175°-180° C. (dec.); 1H NMR D2O, 300 MH...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1CC2CCCN2C1
null
C(Cl)Cl
null
null
Oc1cncc(C23CCCN2CCC3)c1>C(Cl)Cl>Oc1cncc(C23CCCN2CCC3)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d8f9af624c254aa681fb4cd3472eb869
Brc1cncc(Br)c1.C1CC2=[N+](C1)CCC2>>Brc1cncc(C23CCCN2CCC3)c1
BrC=1C=NC=C(C1)Br.[Li]C(C)(C)C.Cl(=O)(=O)(=O)[O-].C1CC[N+]=2CCCC12>>BrC=1C=C(C=NC1)C12CCCN2CCC1
Br[c:6]1[cH:5][n:4][cH:3][c:2]([Br:1])[cH:15]1.[C:7]12=[N+:11]([CH2:10][CH2:9][CH2:8]1)[CH2:12][CH2:13][CH2:14]2>>[Br:1][c:2]1[cH:3][n:4][cH:5][c:6]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[cH:15]1
Brc1cncc(Br)c1.C1CC2=[N+](C1)CCC2
Brc1cncc(C23CCCN2CCC3)c1
null
null
CCCCC
Functional Group Interconversion
OtherReaction
6e757ff9396a07e923211312afac1c080dd23eff3444ff9c846ed5fe9d4243b6
773dbb8365a8bceadef31887b9f43d5f4f5443038ea5ede92ac6bcd66c5d17b4
c1cncc(C23CCCN2CCC3)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1.[C:7]1-[C:8]-[C:9]-[C;H0;D3;+0:10]2=[N+;H0;D3:11]-1-[C:12]-[C:13]-[C:14]-2>>[#7;a:5]1:[c:4]:[c:3]:[c:2]:[c;H0;D3;+0:1](-[C;H0;D4;+0:10]23-[C:14]-[C:13]-[C:12]-[N;H0;D3;+0:11]-2-[C:7]-[C:8]-[C:9]-3):[c:6]:1
28.4
[{"value": 28.0, "product": "BrC=1C=C(C=NC1)C12CCCN2CCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 28.4, "product": "BrC=1C=C(C=NC1)C12CCCN2CCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-95
CELSIUS
null
null
3,5-dibromopyridine (500 mg, 2.11 mmol, Aldrich) was dissolved in Et2 O and cooled to -95° C. A solution of 2.5M t-BuLi (1.7M in pentane, 2.7 mL, 4.64 mmol) in pentane was added dropwise. 1,2,3,5,6,7-hexahydropyrrolizinium perchlorate (663 mg, 3.2 mmol) was added, and the reaction mixture was allowed to stir and warm t...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Tertiary amine
c1ccncc1.C1CC2=[N+](C1)CCC2
c1ccncc1.C1CC2CCCN2C1
c1ccncc1.C1CC2CCCN2C1
Br-
CCCCC
-95
null
Brc1cncc(Br)c1.C1CC2=[N+](C1)CCC2>CCCCC>Brc1cncc(C23CCCN2CCC3)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a1d18582f0384a23a908dc1e462f1ea7
Cl>>Cl
BrC=1C=C(C=NC1)C12CCCN2CCC1.CCOCC.Cl>>Cl.BrC=1C=C(C=NC1)C12CCCN2CCC1
[ClH:16]>>[ClH:16]
Cl
Cl
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
null
null
null
null
7a-(5-bromo-3-pyridinyl)-hexahydro-1H-pyrrolizine (107 mg, 0.52 mmol, from step 16c) was dissolved in methylene chloride, and Et2O saturated with HCl (g) was added. The solvent was removed, and the solid was crystallized from MeOH/Et2O and dried to afford the title compound as an off-white powder (118 mg). mp 192°-194°...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
C(Cl)Cl
null
null
Cl>C(Cl)Cl>Cl