dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
time_units
large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-df24f20e04da4cf9bb28b80952681e46
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3n2C)cc1C=O>>COc1cc(OC)c(-c2cc3ccccc3n2C)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
C(C)(=O)C1=CC=C(C(=O)O)C=C1.COC1=C(C=O)C=C(C(=C1)OC)C=1N(C2=CC=CC=C2C1)C>>COC1=C(C=C(C(=C1)OC)C=1N(C2=CC=CC=C2C1)C)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1
[CH3:22][C:23](=[O:24])[c:25]1[cH:26][cH:27][c:28]([C:29](=[O:30])[OH:31])[cH:32][cH:33]1.O=[CH:21][c:20]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[n:17]2[CH3:18])[cH:19]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:1...
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3n2C)cc1C=O
COc1cc(OC)c(-c2cc3ccccc3n2C)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
null
null
null
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cc3ccccc3[nH]2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
87
[{"value": 87.0, "product": "COC1=C(C=C(C(=C1)OC)C=1N(C2=CC=CC=C2C1)C)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared by condensing 4-acetylbenzoic acid and 2,4-dimethoxy-5-(1-methyl-1H-indol-2-yl)-benzaldehyde (Ex-116A) in a similar manner as described in Ex-3. Yellow solid, 87% yield, mp 157–160° C. 1H-NMR (DMSO-d6) δ 8.17 (d, J=8 Hz, 2H), 8.08 (d, J=15 Hz, 1H), 7.99–9.02 (m 3H), 7.83 (d, J=15 Hz, 1H)...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1cc2ccccc2[nH]1.c1ccccc1
HO-
null
null
null
CC(=O)c1ccc(C(=O)O)cc1.COc1cc(OC)c(-c2cc3ccccc3n2C)cc1C=O>>COc1cc(OC)c(-c2cc3ccccc3n2C)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4008bb8a60f04f23b51dc898f7d8ac43
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(OC)c(-c2cc3ccccc3n2C)cc1C=O>>COc1cc(OC)c(-c2cc3ccccc3n2C)cc1/C=C/C(=O)c1ccc(S(N)(=O)=O)cc1
C(C)(=O)C1=CC=C(C=C1)S(=O)(=O)N.COC1=C(C=O)C=C(C(=C1)OC)C=1N(C2=CC=CC=C2C1)C>>COC1=C(C=C(C(=C1)OC)C=1N(C2=CC=CC=C2C1)C)/C=C/C(=O)C1=CC=C(C=C1)S(=O)(=O)N
[CH3:22][C:23](=[O:24])[c:25]1[cH:26][cH:27][c:28]([S:29]([NH2:30])(=[O:31])=[O:32])[cH:33][cH:34]1.O=[CH:21][c:20]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[n:17]2[CH3:18])[cH:19]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[c...
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(OC)c(-c2cc3ccccc3n2C)cc1C=O
COc1cc(OC)c(-c2cc3ccccc3n2C)cc1/C=C/C(=O)c1ccc(S(N)(=O)=O)cc1
null
null
null
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(-c2cc3ccccc3[nH]2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
90
[{"value": 90.0, "product": "COC1=C(C=C(C(=C1)OC)C=1N(C2=CC=CC=C2C1)C)/C=C/C(=O)C1=CC=C(C=C1)S(=O)(=O)N", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared by condensing 4-acetyl-benzenesulfonamide (Ex-26A) and 2,4-dimethoxy-5-(1-methyl-1H-indol-2-yl)-benzaldehyde (Ex-116A) in a similar manner as described in Ex-3. Yellow solid, 90% yield, mp 148–150° C. 1H-NMR (CDCl3) δ 8.17 (d, J=16 Hz, 1H), 8.09 (d, J=9 Hz, 2H), 8.01 (d, J=9 Hz, 2H), 7.6...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1cc2ccccc2[nH]1.c1ccccc1
HO-
null
null
null
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(OC)c(-c2cc3ccccc3n2C)cc1C=O>>COc1cc(OC)c(-c2cc3ccccc3n2C)cc1/C=C/C(=O)c1ccc(S(N)(=O)=O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-121190dfed7e49c9b66c38f912eb6470
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1>>COC(=O)c1ccc(C(=O)/C=C/c2cc(-c3cc4ccccc4s3)c(OC)cc2OC)cc1
S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C=CC=C2.CCN=C=NCCCN(C)C>>COC(C1=CC=C(C=C1)C(\C=C\C1=C(C=C(C(=C1)C1=CC2=C(S1)C=CC=C2)OC)OC)=O)=O
[OH:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([C:9](=[O:10])/[CH:11]=[CH:12]/[c:13]2[cH:14][c:15](-[c:16]3[cH:17][c:18]4[cH:19][cH:20][cH:21][cH:22][c:23]4[s:24]3)[c:25]([O:26][CH3:27])[cH:28][c:29]2[O:30][CH3:31])[cH:32][cH:33]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([C:9](=[O:10])/[CH:11]=[CH:12]/[c:13]2[cH:1...
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
COC(=O)c1ccc(C(=O)/C=C/c2cc(-c3cc4ccccc4s3)c(OC)cc2OC)cc1
null
CN(C)C=1C=CN=CC1
CO
Miscellaneous
Protection of carboxylic acid
56520e0abb4535dce9a663824ca803b71c2c0dd72dfd246317d953596a987bd2
2ccc7a30191c2c171b49e8a0217bee87430687dd0f567141eca025a75b7e3136
O=C(/C=C/c1cccc(-c2cc3ccccc3s2)c1)c1ccccc1
[O;D1;H0:1]=[C:2](-[OH;D1;+0:3])-[c:4]>>[C;D1;H3:5]-[O;H0;D2;+0:3]-[C:2](=[O;D1;H0:1])-[c:4]
34
[{"value": 34.0, "product": "COC(C1=CC=C(C=C1)C(\\C=C\\C1=C(C=C(C(=C1)C1=CC2=C(S1)C=CC=C2)OC)OC)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared by esterification of 4-[3E-(5-Benzo[b]thiophen-2-yl-2,4-dimethoxy-phenyl)-acryloyl]-benzoic acid (Ex-3) with methanol in the presence of EDCI and DMAP. Yellow solid, 34% yield, m.p. 149–151° C. 1H-NMR (300 MHz, CDCl3): 8.17 (d, 2H, J=6.7 Hz), 8.10 (d, 1H, J=15.8 Hz), 8.05 (d, 2H, J=6.7 H...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ester
null
null
c1ccccc1.c1ccccc1.c1ccc2sccc2c1
Other
CN(C)C=1C=CN=CC1.CO
null
null
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1>CN(C)C=1C=CN=CC1.CO>COC(=O)c1ccc(C(=O)/C=C/c2cc(-c3cc4ccccc4s3)c(OC)cc2OC)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-102420b016204a699014c908bf046c20
C1=COCC1.O=Cc1cccc(Br)c1>>O=Cc1cccc(C2CC=CO2)c1
BrC=1C=CC=C(C=O)C1.O1CCC=C1.C([O-])([O-])=O.[Cs+].[Cs+]>>O1C(CC=C1)C=1C=C(C=O)C=CC1
[CH2:8]1[CH2:9][CH:10]=[CH:11][O:12]1.Br[c:7]1[cH:6][cH:5][cH:4][c:3]([CH:2]=[O:1])[cH:13]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][c:7]([CH:8]2[CH2:9][CH:10]=[CH:11][O:12]2)[cH:13]1
C1=COCC1.O=Cc1cccc(Br)c1
O=Cc1cccc(C2CC=CO2)c1
null
CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C
O.O1CCOCC1
C-C Coupling
OtherReaction
b4051ff7812d7cf0468f49113ffe018c214c07832327c3b42ebcaca827365c2f
3443c4588802a91da83028657a198e0d6619987ecc7555a2d5e93ba54d1cefc1
C1=COC(c2ccccc2)C1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6]:[c:7].[#8:8]1-[C:9]=[C:10]-[C:11]-[CH2;D2;+0:12]-1>>[O;D1;H0:5]=[C:4]-[c:3]:[c:2]:[c;H0;D3;+0:1](-[CH;D3;+0:12]1-[#8:8]-[C:9]=[C:10]-[C:11]-1):[c:6]:[c:7]
40
[{"value": 40.0, "product": "O1C(CC=C1)C=1C=C(C=O)C=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 38.3, "product": "O1C(CC=C1)C=1C=C(C=O)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
45
CELSIUS
null
null
Ex-119A: 5-Bromobenzaldehyde (0.5 g, 2.7 mmol) and 2,3-dihydrofuran (0.56 g, 8.1 mmol) were dissolved in dioxane (5.0 mL). Nitrogen was bubbled into the solution for 15 min followed by the sequential addition of cesium carbonate (0.96 g, 2.9 mmol) and bis(tri-t-butylphosphine)palladium(0) (0.014 g, 0.027 mmol). The sol...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ether
Ether
C1=COCC1.c1ccccc1
c1ccccc1.C1=COCC1
c1ccccc1.C1=COCC1
HBr
CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C.O.O1CCOCC1
45
null
C1=COCC1.O=Cc1cccc(Br)c1>CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C.O.O1CCOCC1>O=Cc1cccc(C2CC=CO2)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ed4268e224394520a5276dcd202bcc05
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1>>COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C=CC=C2.C(C)O.C(C)O.S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C=CC=C2.CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO.N(C)C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO>>CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO.S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O...
[CH3:14][O:15][c:16]1[cH:17][c:18]([O:19][CH3:20])[c:21](-[c:22]2[cH:23][c:24]3[cH:25][cH:26][cH:27][cH:28][c:29]3[s:30]2)[cH:31][c:32]1/[CH:33]=[CH:34]/[C:35](=[O:36])[c:37]1[cH:38][cH:39][c:40]([C:41](=[O:42])[OH:43])[cH:44][cH:45]1>>[CH3:14][O:15][c:16]1[cH:17][c:18]([O:19][CH3:20])[c:21](-[c:22]2[cH:23][c:24]3[cH:2...
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
null
null
C1CCOC1
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
O=C(/C=C/c1cccc(-c2cc3ccccc3s2)c1)c1ccccc1
null
63
[{"value": 63.0, "product": "CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO.S1C2=C(C=C1C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C(=O)O)C=C1)OC)OC)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
4-[3E-(5-Benzo[b]thien-2-yl-2,4-dimethoxyphenyl)-acryloyl]-benzoic acid of Ex. 3 was then made into a meglumine salt by suspending the 4-[3E-(5-benzo[b]thien-2-yl-2,4-dimethoxy-phenyl)-acryloyl]-benzoic acid (4.45 g, 10 mmol) and N-methyl-D-glucamine (1.95 g, 10 mmol) in THF (100 mL). The mixture was stirred at room te...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1ccc2sccc2c1.c1ccccc1
null
C1CCOC1
null
0.083333
COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1>C1CCOC1>COc1cc(OC)c(-c2cc3ccccc3s2)cc1/C=C/C(=O)c1ccc(C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6afee8efff1c471f86bb728d2c260d3f
C1=COCC1.COc1cc(OC)c(C=O)cc1Br>>COc1cc(OC)c(C2C=CCO2)cc1C=O
BrC=1C(=CC(=C(C=O)C1)OC)OC.O1CCC=C1.C([O-])([O-])=O.[Cs+].[Cs+].C([O-])([O-])=O.[Cs+].[Cs+].O1CCC=C1>>O1C(C=CC1)C=1C(=CC(=C(C=O)C1)OC)OC
[CH:9]1=[CH:10][CH2:11][CH2:12][O:13]1.Br[c:8]1[c:5]([O:6][CH3:7])[cH:4][c:3]([O:2][CH3:1])[c:15]([CH:16]=[O:17])[cH:14]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8]([CH:9]2[CH:10]=[CH:11][CH2:12][O:13]2)[cH:14][c:15]1[CH:16]=[O:17]
C1=COCC1.COc1cc(OC)c(C=O)cc1Br
COc1cc(OC)c(C2C=CCO2)cc1C=O
null
CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C.[Pd]
O.O1CCOCC1
C-C Coupling
OtherReaction
413b6e05569e921eef7402c1b4571776ae22bc64b64a6ffc6f42f3ccfc1a789e
3443c4588802a91da83028657a198e0d6619987ecc7555a2d5e93ba54d1cefc1
C1=CC(c2ccccc2)OC1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]-[C:4]=[O;D1;H0:5]):[c:6](-[#8:7]):[c:8].[#8:9]1-[C:10]-[CH2;D2;+0:11]-[CH;D2;+0:12]=[CH;D2;+0:13]-1>>[#8:7]-[c:6](:[c:8]):[c;H0;D3;+0:1](-[CH;D3;+0:13]1-[#8:9]-[C:10]-[CH;D2;+0:11]=[CH;D2;+0:12]-1):[c:2]:[c:3]-[C:4]=[O;D1;H0:5]
50
[{"value": 50.0, "product": "O1C(C=CC1)C=1C(=CC(=C(C=O)C1)OC)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 34.2, "product": "O1C(C=CC1)C=1C(=CC(=C(C=O)C1)OC)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
45
CELSIUS
null
null
Ex-121A: 5-Bromo-2,4-dimethoxybenzaldehyde (1.0 g, 4.0 mmol) and 2,3-dihydrofuran (0.85 g, 12.2 mmol) were dissolved in dioxane (10.0 mL). Nitrogen was bubbled into the solution for 15 min followed by the sequential addition of cesium carbonate (1.4 g, 4.5 mmol) and bis(tri-t-butylphosphine)palladium (0) (0.021 g, 0.04...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ether
Ether
C1=COCC1.c1ccccc1
c1ccccc1.C1=CCOC1
c1ccccc1.C1=CCOC1
HBr
CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C.[Pd].O.O1CCOCC1
45
null
C1=COCC1.COc1cc(OC)c(C=O)cc1Br>CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C.[Pd].O.O1CCOCC1>COc1cc(OC)c(C2C=CCO2)cc1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5e15b01335cb4372a6985500921ddfea
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(OC)c(C2C=CCO2)cc1C=O>>COc1cc(OC)c(C2C=CCO2)cc1/C=C/C(=O)c1ccc(S(N)(=O)=O)cc1
O1C(C=CC1)C=1C(=CC(=C(C=O)C1)OC)OC.C(C)(=O)C1=CC=C(C=C1)S(=O)(=O)N.C[O-].[Li+]>>O1C(C=CC1)C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C=C1)S(=O)(=O)N)OC)OC
[CH3:17][C:18](=[O:19])[c:20]1[cH:21][cH:22][c:23]([S:24]([NH2:25])(=[O:26])=[O:27])[cH:28][cH:29]1.O=[CH:16][c:15]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8]([CH:9]2[CH:10]=[CH:11][CH2:12][O:13]2)[cH:14]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8]([CH:9]2[CH:10]=[CH:11][CH2:12][O:13]2)[cH:14][c:15]1/[CH:...
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(OC)c(C2C=CCO2)cc1C=O
COc1cc(OC)c(C2C=CCO2)cc1/C=C/C(=O)c1ccc(S(N)(=O)=O)cc1
null
null
O.CN(C=O)C.CO
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cccc(C2C=CCO2)c1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
72.8
[{"value": 70.0, "product": "O1C(C=CC1)C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C=C1)S(=O)(=O)N)OC)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 72.8, "product": "O1C(C=CC1)C=1C(=CC(=C(C1)/C=C/C(=O)C1=CC=C(C=C1)S(=O)(=O)N)OC)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
5-(2,5-Dihydro-furan-2-yl)-2,4-dimethoxy-benzaldehyde (Ex-121A, 0.10 g, 0.43 mmol) and 4-acetylbenzenesulfonamide (Ex-26A, 0.085 g, 0.43 mmol) were dissolved in a dimethylformamide-methanol solution (2.9 mL, 7:3). After complete dissolution, lithium methoxide (0.065 g, 1.7 mmol) was added and the resulting orange slurr...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.C1=CCOC1.c1ccccc1
HO-
O.CN(C=O)C.CO
null
4
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(OC)c(C2C=CCO2)cc1C=O>O.CN(C=O)C.CO>COc1cc(OC)c(C2C=CCO2)cc1/C=C/C(=O)c1ccc(S(N)(=O)=O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bf7cac834a044372bd0d04983d7dc8e9
COc1cc(O)c(C=O)cc1-c1cccs1.Cc1cccc(Br)n1>>COc1cc(Oc2cccc(C)n2)c(C=O)cc1-c1cccs1
[O-]C1=CC=CC=C1.C([O-])([O-])=O.[Cs+].[Cs+].OC1=C(C=O)C=C(C(=C1)OC)C=1SC=CC1.BrC1=NC(=CC=C1)C.C1(=CC=CC2=CC=CC=C12)C(=O)O.C([O-])([O-])=O.[Cs+].[Cs+]>>COC1=CC(=C(C=O)C=C1C=1SC=CC1)OC1=NC(=CC=C1)C
[CH3:1][O:2][c:3]1[cH:4][c:5]([OH:6])[c:14]([CH:15]=[O:16])[cH:17][c:18]1-[c:19]1[cH:20][cH:21][cH:22][s:23]1.Br[c:7]1[cH:8][cH:9][cH:10][c:11]([CH3:12])[n:13]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][c:7]2[cH:8][cH:9][cH:10][c:11]([CH3:12])[n:13]2)[c:14]([CH:15]=[O:16])[cH:17][c:18]1-[c:19]1[cH:20][cH:21][cH:22][s:23]1
COc1cc(O)c(C=O)cc1-c1cccs1.Cc1cccc(Br)n1
COc1cc(Oc2cccc(C)n2)c(C=O)cc1-c1cccs1
null
null
C(C)(=O)OCC.[OH-].[Na+].C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
99925b30dd2603ae575cba81b58435d015cd6b7267cf347380904f25833af5f2
27e9a6bab4e3ed54aeb6be4d84cb1c0170208288795e252a46e57e44ecc064f0
c1ccc(Oc2ccc(-c3cccs3)cc2)nc1
Br-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5].[O;D1;H0:6]=[C:7]-[c:8]:[c:9](-[OH;D1;+0:10]):[c:11]>>[O;D1;H0:6]=[C:7]-[c:8]:[c:9](-[O;H0;D2;+0:10]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5]):[c:11]
65.9
[{"value": 65.0, "product": "COC1=CC(=C(C=O)C=C1C=1SC=CC1)OC1=NC(=CC=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 65.9, "product": "COC1=CC(=C(C=O)C=C1C=1SC=CC1)OC1=NC(=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
110
CELSIUS
null
null
Ex-122A: To a solution of 2-hydroxy-4-methoxy-5-thiophen-2-yl-benzaldehyde (0.68 g, 2.9 mmol) and 2-bromo-6-methylpyridine (0.25 g, 1.4 mmol) in toluene (1.0 mL) was added ethyl acetate (0.0063 g, 0.072 mmol, 1-naphthoic acid (0.50 g, 2.9 mmol), 5 Å molecular sieves (0.36 g), cesium carbonate (0.94 g, 2.9 mmol), and co...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic alcohol
Ether
c1ccncc1
c1ccncc1
c1ccccc1.c1ccncc1.c1ccsc1
HBr
C(C)(=O)OCC.[OH-].[Na+].C1(=CC=CC=C1)C
110
null
COc1cc(O)c(C=O)cc1-c1cccs1.Cc1cccc(Br)n1>C(C)(=O)OCC.[OH-].[Na+].C1(=CC=CC=C1)C>COc1cc(Oc2cccc(C)n2)c(C=O)cc1-c1cccs1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0a7cdf7bc4c84be6b16e9755a8d7b988
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(Oc2cccc(C)n2)c(C=O)cc1-c1cccs1>>COc1cc(Oc2cccc(C)n2)c(/C=C/C(=O)c2ccc(S(N)(=O)=O)cc2)cc1-c1cccs1
COC1=CC(=C(C=O)C=C1C=1SC=CC1)OC1=NC(=CC=C1)C.C(C)(=O)C1=CC=C(C=C1)S(=O)(=O)N.C[O-].[Li+]>>COC1=CC(=C(C=C1C=1SC=CC1)/C=C/C(=O)C1=CC=C(C=C1)S(=O)(=O)N)OC1=NC(=CC=C1)C
[CH3:16][C:17](=[O:18])[c:19]1[cH:20][cH:21][c:22]([S:23]([NH2:24])(=[O:25])=[O:26])[cH:27][cH:28]1.O=[CH:15][c:14]1[c:5]([O:6][c:7]2[cH:8][cH:9][cH:10][c:11]([CH3:12])[n:13]2)[cH:4][c:3]([O:2][CH3:1])[c:30](-[c:31]2[cH:32][cH:33][cH:34][s:35]2)[cH:29]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][c:7]2[cH:8][cH:9][cH:10][c:11...
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(Oc2cccc(C)n2)c(C=O)cc1-c1cccs1
COc1cc(Oc2cccc(C)n2)c(/C=C/C(=O)c2ccc(S(N)(=O)=O)cc2)cc1-c1cccs1
null
null
O.CN(C=O)C.CO
C-C Coupling
Aldehyde and ketone to alpha,beta-unsaturated carbonyl
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(/C=C/c1cc(-c2cccs2)ccc1Oc1ccccn1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:7]=[C:6](-[c:8])/[CH;D2;+0:5]=[CH;D2;+0:1]/[c:2](:[c:3]):[c:4]
82
[{"value": 82.0, "product": "COC1=CC(=C(C=C1C=1SC=CC1)/C=C/C(=O)C1=CC=C(C=C1)S(=O)(=O)N)OC1=NC(=CC=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.6, "product": "COC1=CC(=C(C=C1C=1SC=CC1)/C=C/C(=O)C1=CC=C(C=C1)S(=O)(=O)N)OC1=NC(=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
4-Methoxy-2-(6-methyl-pyridin-2-yloxy)-5-thiophen-2-yl-benzaldehyde (Ex-122A, 0.20 g, 0.62 mmol) and 4-acetylbenzenesulfonamide (Ex-26A, 0.12 g, 0.62 mmol) were dissolved in a dimethylformamide-methanol solution (4.2 mL, 7:3). After complete dissolution, lithium methoxide (0.093 g, 2.5 mmol) was added and the resulting...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccncc1.c1ccccc1.c1ccsc1
HO-
O.CN(C=O)C.CO
null
3
CC(=O)c1ccc(S(N)(=O)=O)cc1.COc1cc(Oc2cccc(C)n2)c(C=O)cc1-c1cccs1>O.CN(C=O)C.CO>COc1cc(Oc2cccc(C)n2)c(/C=C/C(=O)c2ccc(S(N)(=O)=O)cc2)cc1-c1cccs1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e6aaf19072de4abd8400219da961b065
COc1ccc(C=O)c(OC)c1.ClI>>COc1cc(OC)c(C=O)cc1I
COC1=C(C=O)C=CC(=C1)OC.ICl.Cl>>IC=1C(=CC(=C(C=O)C1)OC)OC
[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8]([CH:9]=[O:10])[cH:11][cH:12]1.Cl[I:13]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8]([CH:9]=[O:10])[cH:11][c:12]1[I:13]
COc1ccc(C=O)c(OC)c1.ClI
COc1cc(OC)c(C=O)cc1I
null
null
CO
Functional Group Interconversion
OtherReaction
f6effe61353895b318215d8bd9b6bb1105cafbf7be8c217d748df587260b32c3
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccccc1
Cl-[I;H0;D1;+0:1].[#8:2]-[c:3](:[c:4]):[cH;D2;+0:5]:[c:6]:[c:7]-[C:8]=[O;D1;H0:9]>>[#8:2]-[c:3](:[c:4]):[c;H0;D3;+0:5](-[I;H0;D1;+0:1]):[c:6]:[c:7]-[C:8]=[O;D1;H0:9]
87.5
[{"value": 87.5, "product": "IC=1C(=CC(=C(C=O)C1)OC)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.1, "product": "IC=1C(=CC(=C(C=O)C1)OC)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a solution of 2,4-dimethoxy-benzaldehyde (20.0 g, 120.4 mmol) in methanol (550 mL) was added a solution of iodine monochloride (23.25 g, 144.9 mmol) in methanol (60 mL) dropwise over 20 min. The solution was allowed to stir at ambient temperature for 3 hours and then poured into a solution of hydrochloric acid (0.5 ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccccc1
c1ccccc1
c1ccccc1
HCl
CO
null
3
COc1ccc(C=O)c(OC)c1.ClI>CO>COc1cc(OC)c(C=O)cc1I
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b7422b77623e43858abc2bb907b837a8
COc1cc(OC)c(C=O)cc1I.OB(O)c1cc2ccccc2s1>>COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
[F-].[K+].IC=1C(=CC(=C(C=O)C1)OC)OC.S1C2=C(C=C1B(O)O)C=CC=C2.C(C)(C)(C)P(C(C)(C)C)C(C)(C)C.IC=1C(=CC(=C(C=O)C1)OC)OC>>S1C2=C(C=C1C=1C(=CC(=C(C=O)C1)OC)OC)C=CC=C2
I[c:19]1[c:3]([O:2][CH3:1])[cH:4][c:5]([O:6][CH3:7])[c:8]([CH:20]=[O:21])[cH:18]1.OB(O)[c:9]1[cH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[s:17]1>>[CH3:1][O:2][c:3]1[cH:4][c:5]([O:6][CH3:7])[c:8](-[c:9]2[cH:10][c:11]3[cH:12][cH:13][cH:14][cH:15][c:16]3[s:17]2)[cH:18][c:19]1[CH:20]=[O:21]
COc1cc(OC)c(C=O)cc1I.OB(O)c1cc2ccccc2s1
COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
null
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd]
O1CCCC1
C-C Coupling
Suzuki coupling with boronic acids
15493b37b8243b24918da50e88da7a22606e9a543d93422d66b895008aa4e97c
743f778b861da0302c62360b1c4b2edc21b2c3696b81449369faeaaeab501dbc
c1ccc(-c2cc3ccccc3s2)cc1
I-[c;H0;D3;+0:1]1:[c:2]:[c;H0;D3;+0:3](-[CH;D2;+0:4]=[O;D1;H0:5]):[c:6](-[#8:7]):[c:8]:[c:9]:1-[#8:10].O-B(-O)-[c;H0;D3;+0:11]1:[#16;a:12]:[c:13]:[c:14]:[c:15]:1>>[#8:10]-[c:9]1:[c:8]:[c:6](-[#8:7]):[c;H0;D3;+0:3](-[c;H0;D3;+0:11]2:[#16;a:12]:[c:13]:[c:14]:[c:15]:2):[c:2]:[c;H0;D3;+0:1]:1-[CH;D2;+0:4]=[O;D1;H0:5]
null
[]
60
CELSIUS
null
null
Ex-123A: Potassium fluoride (0.42 g, 7.2 mmol), 5-iodo-2,4-dimethoxy-benzaldehyde (Ex-123, 1.0 g, 3.42 mmol), 2-benzo[b]thiophene boronic acid (0.67 g, 3.77 mmol), degased tetrahydrofuran (10 mL), tris(dibenzylideneacetone)dipalladium (19 mg, 0.02 mmol), and tri-tert-butylphosphine (100 mg, 0.05 mmol) were sequentially...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aldehyde.Boronic acid
Aldehyde
c1ccccc1.c1ccc2sccc2c1
c1ccccc1.c1ccc2sccc2c1
c1ccccc1.c1ccc2sccc2c1
HI.B
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].O1CCCC1
60
null
COc1cc(OC)c(C=O)cc1I.OB(O)c1cc2ccccc2s1>C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].O1CCCC1>COc1cc(OC)c(-c2cc3ccccc3s2)cc1C=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-868789ba44d24a379570d31b85128dc2
NN.O=[N+]([O-])c1cc(C(F)(F)F)ccc1Cl>>On1nnc2ccc(C(F)(F)F)cc21
ClC1=C(C=C(C=C1)C(F)(F)F)[N+](=O)[O-].O.NN>>ON1N=NC2=C1C=C(C=C2)C(F)(F)F
[NH2:3][NH2:4].[O-][N+:2](=[O:1])[c:14]1[c:5](Cl)[cH:6][cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[cH:13]1>>[OH:1][n:2]1[n:3][n:4][c:5]2[cH:6][cH:7][c:8]([C:9]([F:10])([F:11])[F:12])[cH:13][c:14]12
NN.O=[N+]([O-])c1cc(C(F)(F)F)ccc1Cl
On1nnc2ccc(C(F)(F)F)cc21
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
7782c5939184dde3a46439ac85e20224c3ad846fa2633d412f760cf18c068c41
6c13d8453d798e86c74ea5b8e76450673bfcfa8a64f81673730723d26d8a44f7
c1ccc2[nH]nnc2c1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[N+;H0;D3:5](-[O-])=[O;H0;D1;+0:6]):[c:7].[NH2;D1;+0:8]-[NH2;D1;+0:9]>>[OH;D1;+0:6]-[n;H0;D3;+0:5]1:[n;H0;D2;+0:8]:[n;H0;D2;+0:9]:[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:1:[c:7]
89.5
[{"value": 89.5, "product": "ON1N=NC2=C1C=C(C=C2)C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound is prepared according to the procedure described by K. Takeda [J. Org. Chem., 50, 273, (1985)]. A mixture of 4-chloro-3-nitro-α,α,α-trifluorotoluene (50.0 g, 0.22 moles) and hydrazine hydrate (33.0, 0.33 moles) in absolute ethanol (75 ml) is refluxed for 24 h. After removal of the solvent under reduc...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Aromatic halide.Nitro group
null
c1ccccc1
c1ccc2nn[nH]c2c1
c1ccc2nn[nH]c2c1
HCl
C(C)O
null
null
NN.O=[N+]([O-])c1cc(C(F)(F)F)ccc1Cl>C(C)O>On1nnc2ccc(C(F)(F)F)cc21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ffec451764134a1db4236c62aaba0bd9
CC(=O)CCC(=O)O.CC(C)N=C=NC(C)C>>CCN(C(C)C)C(C)C
C(CCC(=O)C)(=O)O.CC(N=C=NC(C)C)C.C(Cl)Cl>>CCN(C(C)C)C(C)C
O=C(O)CCC(=O)[CH3:1].N(C([CH3:5])[CH3:6])=[C:4]=[N:3][CH:7]([CH3:8])[CH3:9]>>[CH3:1][CH2:2][N:3]([CH:4]([CH3:5])[CH3:6])[CH:7]([CH3:8])[CH3:9]
CC(=O)CCC(=O)O.CC(C)N=C=NC(C)C
CCN(C(C)C)C(C)C
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
d52d66f4d1f27d3af58f45752829cc7ce71f2866d14fa1307908438015cf7969
2f72a54a0c44eacd3ec84f33e577f211923309990de7cce0a6eaf1c53d41f642
null
O-C(=O)-C-C-C(=O)-[CH3;D1;+0:1].[C;D1;H3:2]-[C:3](-[C;D1;H3:4])-[N;H0;D2;+0:5]=[C;H0;D2;+0:6]=N-C(-[CH3;D1;+0:7])-[CH3;D1;+0:8]>>[C;D1;H3:2]-[C:3](-[C;D1;H3:4])-[N;H0;D3;+0:5](-[C:9]-[CH3;D1;+0:1])-[CH;D3;+0:6](-[CH3;D1;+0:7])-[CH3;D1;+0:8]
null
[]
null
null
null
null
addition of activated levulinic acid (activated as the symmetric anhydride with 0.5 equivalents of DIC in DCM for 5-10 min) Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ketone
Tertiary amine
null
null
null
HO-
null
null
null
CC(=O)CCC(=O)O.CC(C)N=C=NC(C)C>>CCN(C(C)C)C(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ebb811057e7d4e2089d709387e100252
O=C(Cl)OCc1ccccc1.O=C(O)C1CCNCC1>>O=C(O)C1CCN(C(=O)OCc2ccccc2)CC1
C(C1=CC=CC=C1)OC(=O)Cl.C(=O)(OCC1=CC=CC=C1)N1CCC(C(=O)O)CC1.N1CCC(C(=O)O)CC1.C([O-])(O)=O.[Na+]>>C(=O)(OCC1=CC=CC=C1)N1CCC(C(=O)O)CC1
Cl[C:8](=[O:9])[O:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1.[O:1]=[C:2]([OH:3])[CH:4]1[CH2:5][CH2:6][NH:7][CH2:18][CH2:19]1>>[O:1]=[C:2]([OH:3])[CH:4]1[CH2:5][CH2:6][N:7]([C:8](=[O:9])[O:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[CH2:18][CH2:19]1
O=C(Cl)OCc1ccccc1.O=C(O)C1CCNCC1
O=C(O)C1CCN(C(=O)OCc2ccccc2)CC1
null
null
O.C1(=CC=CC=C1)C
Protection
N-alkylation of secondary amines with alkyl halides
c6eb958652ca8104567d61601fc03a9cfee33fb7bb328952993831b03fec41c4
d86dc1e6d0e089b3444b62ddfcf4c4822bdac4b60e628553036562518c29adcd
O=C(OCc1ccccc1)N1CCCCC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C:4].[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]>>[C:4]-[#8:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:7](-[C:6]-[C:5])-[C:8]-[C:9]
86
[{"value": 86.0, "product": "C(=O)(OCC1=CC=CC=C1)N1CCC(C(=O)O)CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 74.6, "product": "C(=O)(OCC1=CC=CC=C1)N1CCC(C(=O)O)CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
14
HOUR
N-CBZ-isonipecotic acid Benzyl chloroformate (16.4 mL, 115 mmol) in toluene (50 mL) was added dropwise to a stirred solution of 12.9 g (100 mmol) of isonipecotic acid (Aldrich) and 21.0 g (250 mmol) of sodium bicarbonate in 200 mL of water. After 14 h, the mixture was extracted with ether (3×50 ml) and the ether layers...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether.Secondary amine
Carbamic ester
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccccc1
HCl
O.C1(=CC=CC=C1)C
null
14
O=C(Cl)OCc1ccccc1.O=C(O)C1CCNCC1>O.C1(=CC=CC=C1)C>O=C(O)C1CCN(C(=O)OCc2ccccc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-040a36dbcef644d3b7a53d23ebd88f75
CCOC(=O)CC(=O)OCC.Cc1ccc(Br)c(F)c1>>CCOC(=O)C(C(=O)OCC)c1ccc(C)cc1F
C(CC(=O)OCC)(=O)OCC.[H-].[Na+].BrC1=C(C=C(C=C1)C)F.Cl>>FC1=C(C=CC(=C1)C)C(C(=O)OCC)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:7](=[O:8])[O:9][CH2:10][CH3:11].Br[c:12]1[cH:13][cH:14][c:15]([CH3:16])[cH:17][c:18]1[F:19]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([C:7](=[O:8])[O:9][CH2:10][CH3:11])[c:12]1[cH:13][cH:14][c:15]([CH3:16])[cH:17][c:18]1[F:19]
CCOC(=O)CC(=O)OCC.Cc1ccc(Br)c(F)c1
CCOC(=O)C(C(=O)OCC)c1ccc(C)cc1F
null
null
O1CCOCC1
C-C Coupling
Hurtley reaction
5a1171068c2a10d196160f01101b1c97354196d6923cfc455c6b686284d6c6f2
c0fb657475d92a5e1ab643a3f03921ebe4d047c8d805f98b012a5df3f9fb1f6c
c1ccccc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[F;D1;H0:5]):[c:6].[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH2;D2;+0:11]-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH;D3;+0:11](-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[F;D1;H0:5]):[c:6]
59.6
[{"value": 59.6, "product": "FC1=C(C=CC(=C1)C)C(C(=O)OCC)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
10
MINUTE
0.49 mol of diethyl malonate was added at 60° C. inside 2 hours to a mixture of 0.51 mol of NaH and 140 ml of 1,4-dioxane. The mixture was stirred for approximately 10 min at 60° C. and then 0.05 mol of Cu(I)Br was added. After 15 min, a mixture of 0.25 mol of 4-bromo-3-fluorotoluene and 10 ml of 1,4-dioxane was added....
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ester.Ester
Ester.Ester
c1ccccc1
c1ccccc1
c1ccccc1
HBr
O1CCOCC1
60
0.166667
CCOC(=O)CC(=O)OCC.Cc1ccc(Br)c(F)c1>O1CCOCC1>CCOC(=O)C(C(=O)OCC)c1ccc(C)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f4cfd8c165894839adb182360ea432e1
CC(=O)Nc1ccc(/C=C/C(=O)O)cn1.Cc1ccc2cccc(OCc3c(Cl)ccc(N(C)C(=O)CN)c3Cl)c2n1>>CC(=O)Nc1ccc(/C=C/C(=O)NCC(=O)N(C)c2ccc(Cl)c(COc3cccc4ccc(C)nc34)c2Cl)cn1
NCC(=O)N(C)C=1C(=C(COC=2C=CC=C3C=CC(=NC23)C)C(=CC1)Cl)Cl.C(C)(=O)NC1=CC=C(C=N1)/C=C/C(=O)O.ON1N=NC2=C1C=CC=C2.Cl.C(C)N=C=NCCCN(C)C>>C(C)(=O)NC1=CC=C(C=N1)/C=C/C(=O)NCC(=O)N(C)C=1C(=C(COC=2C=CC=C3C=CC(=NC23)C)C(=CC1)Cl)Cl
O[C:11](/[CH:10]=[CH:9]/[c:8]1[cH:7][cH:6][c:5]([NH:4][C:2]([CH3:1])=[O:3])[n:41][cH:40]1)=[O:12].[NH2:13][CH2:14][C:15](=[O:16])[N:17]([CH3:18])[c:19]1[cH:20][cH:21][c:22]([Cl:23])[c:24]([CH2:25][O:26][c:27]2[cH:28][cH:29][cH:30][c:31]3[cH:32][cH:33][c:34]([CH3:35])[n:36][c:37]23)[c:38]1[Cl:39]>>[CH3:1][C:2](=[O:3])[N...
CC(=O)Nc1ccc(/C=C/C(=O)O)cn1.Cc1ccc2cccc(OCc3c(Cl)ccc(N(C)C(=O)CN)c3Cl)c2n1
CC(=O)Nc1ccc(/C=C/C(=O)NCC(=O)N(C)c2ccc(Cl)c(COc3cccc4ccc(C)nc34)c2Cl)cn1
null
null
O.CN(C=O)C
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(/C=C/c1cccnc1)NCC(=O)Nc1cccc(COc2cccc3cccnc23)c1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])/[C:3]=[C:4]/[c:5](:[c:6]):[c:7]:[#7;a:8].[C;D1;H3:9]-[#7:10](-[c:11])-[C:12](=[O;D1;H0:13])-[C:14]-[NH2;D1;+0:15]>>[#7;a:8]:[c:7]:[c:5](/[C:4]=[C:3]/[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:15]-[C:14]-[C:12](=[O;D1;H0:13])-[#7:10](-[C;D1;H3:9])-[c:11]):[c:6]
53.8
[{"value": 53.8, "product": "C(C)(=O)NC1=CC=C(C=N1)/C=C/C(=O)NCC(=O)N(C)C=1C(=C(COC=2C=CC=C3C=CC(=NC23)C)C(=CC1)Cl)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a mixture of 8-[3-(N-glycyl-N-methylamino)-2,6-dichlorobenzyloxy]-2-methylquinoline (100 mg), (E)-3-(6-acetamidopyridin-3-yl)acrylic acid (56.1 mg) and N,N-dimethylformamide (2 ml) were added 1-hydroxybenzotriazole (43.4 mg) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (56.9 mg) in a nitrogen stre...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccncc1.c1ccccc1.c1ccc2ncccc2c1
HO-
O.CN(C=O)C
null
2
CC(=O)Nc1ccc(/C=C/C(=O)O)cn1.Cc1ccc2cccc(OCc3c(Cl)ccc(N(C)C(=O)CN)c3Cl)c2n1>O.CN(C=O)C>CC(=O)Nc1ccc(/C=C/C(=O)NCC(=O)N(C)c2ccc(Cl)c(COc3cccc4ccc(C)nc34)c2Cl)cn1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c6da0580259c4980b9f5ec2af98dfe19
O=C(CCl)CCl.c1nc[nH]n1>>O=C(Cn1cncn1)Cn1cncn1
ClCC(=O)CCl.N1N=CN=C1>>N1(N=CN=C1)CC(CN1N=CN=C1)=O
Cl[CH2:3][C:2](=[O:1])[CH2:5]Cl.[n:4]1[nH:10][cH:11][n:12][cH:13]1>>[O:1]=[C:2]([CH2:3][n:4]1[cH:5][n:6][cH:7][n:8]1)[CH2:9][n:10]1[cH:11][n:12][cH:13][n:14]1
O=C(CCl)CCl.c1nc[nH]n1
O=C(Cn1cncn1)Cn1cncn1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
90bae339f52889fdabd8686acc1edf342b27a03a66f2d05c7a8a9253bdeb0552
277d117055f0fa9c0a7b0fdec46e3e097718c606328ceb6568d2848aeec088a0
O=C(Cn1cncn1)Cn1cncn1
Cl-[CH2;D2;+0:1]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[CH2;D2;+0:4]-Cl.[#7;a:5]1:[c:6]:[nH;D2;+0:7]:[n;H0;D2;+0:8]:[cH;D2;+0:9]:1>>[O;D1;H0:3]=[C;H0;D3;+0:2](-[C:10]-[n;H0;D3;+0:7]1:[#7;a:11]:[cH;D2;+0:9]:[#7;a:5]:[c:6]:1)-[CH2;D2;+0:1]-[n;H0;D3;+0:8]1:[#7;a:12]:[c:13]:[#7;a:14]:[cH;D2;+0:4]:1
null
[]
null
null
null
null
According to the Spanish Patent Number ES 549 020 A1 1 mole of 1,3-dichloroacetone is reacted with 2 mole of 1,2,4-triazole, then the 1,3-bis(1,2,4-triazole-1-yl)-propan-2-on obtained with low yield is reacted with 2,4-difluorophenylmagnesium bromide to give fluconazole. The yield is about 45% calculated on the Grignar...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Ketone
Ketone
c1nc[nH]n1
c1nc[nH]n1.c1nc[nH]n1
c1nc[nH]n1.c1nc[nH]n1
null
null
null
null
O=C(CCl)CCl.c1nc[nH]n1>>O=C(Cn1cncn1)Cn1cncn1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-62a977a3af3043749e5018d7d27db422
CO.C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F>>O.OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
FC1=C(C=CC(=C1)F)C(CN1N=CN=C1)(CN1N=CN=C1)O[Si](C)(C)C.CO.Cl>>O.FC1=C(C=CC(=C1)F)C(CN1N=CN=C1)(CN1N=CN=C1)O
C[OH:1].C[Si](C)(C)[O:2][C:3]([CH2:4][n:5]1[cH:6][n:7][cH:8][n:9]1)([CH2:10][n:11]1[cH:12][n:13][cH:14][n:15]1)[c:16]1[cH:17][cH:18][c:19]([F:20])[cH:21][c:22]1[F:23]>>[OH2:1].[OH:2][C:3]([CH2:4][n:5]1[cH:6][n:7][cH:8][n:9]1)([CH2:10][n:11]1[cH:12][n:13][cH:14][n:15]1)[c:16]1[cH:17][cH:18][c:19]([F:20])[cH:21][c:22]1[F...
CO.C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
O.OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
null
null
O
Miscellaneous
OtherReaction
357eac61f447b32e729168579f8528da7da26588dfc2d31885d5df9d98532f35
844fd118cb6d4293b2696a11189831ba9ccdbbec968ff2a96f22a1fed914fdaf
c1ccc(C(Cn2cncn2)Cn2cncn2)cc1
C-[OH;D1;+0:1].C-[Si](-C)(-C)-[O;H0;D2;+0:2]-[C:3](-[C:4])(-[C:5])-[c:6]>>[C:4]-[C:3](-[C:5])(-[OH;D1;+0:2])-[c:6].[OH2;D0;+0:1]
186.9
[{"value": 93.5, "product": "O.FC1=C(C=CC(=C1)F)C(CN1N=CN=C1)(CN1N=CN=C1)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 186.9, "product": "O.FC1=C(C=CC(=C1)F)C(CN1N=CN=C1)(CN1N=CN=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 7.50 g (0.02 mol) of 2-(2,4-difluorophenyl)-1,3-bis(1,2,4-triazole-1-yl)-2-(trimethylsilyloxy)propane, 25 ml of methanol, 2 ml of water and 1.0 ml of concd. hydrochloric acid was stirred at 30° C. for 1 h. The reaction mixture was concentrated to a volume of 10 ml and after adding 50 ml of water the pH of ...
10.6084/m9.figshare.5104873.v1
null
Methanol.Silyl protective group
Tertiary alcohol
null
null
c1nc[nH]n1.c1nc[nH]n1.c1ccccc1
Other
O
null
null
CO.C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F>O>O.OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2b91f17c041f48b492f8978539c07591
C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F>>OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
FC1=C(C=CC(=C1)F)C(CN1N=CN=C1)(CN1N=CN=C1)O[Si](C)(C)C.CO.[OH-].[Na+]>>C1=CC(=C(C=C1F)F)C(CN2C=NC=N2)(CN3C=NC=N3)O
C[Si](C)(C)[O:1][C:2]([CH2:3][n:4]1[cH:5][n:6][cH:7][n:8]1)([CH2:9][n:10]1[cH:11][n:12][cH:13][n:14]1)[c:15]1[cH:16][cH:17][c:18]([F:19])[cH:20][c:21]1[F:22]>>[OH:1][C:2]([CH2:3][n:4]1[cH:5][n:6][cH:7][n:8]1)([CH2:9][n:10]1[cH:11][n:12][cH:13][n:14]1)[c:15]1[cH:16][cH:17][c:18]([F:19])[cH:20][c:21]1[F:22]
C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
null
null
O
Deprotection
Alcohol deprotection from silyl ethers
6d1f3bf0e00171fd9431270b3a5c35c615a5f2d97feae7c0a7b6dc8ba859d8aa
bf9cbf8f6c3a5d5e13b674dc7a2b872a6c60a00401e068847221a255cbca9558
c1ccc(C(Cn2cncn2)Cn2cncn2)cc1
C-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])(-[C:4])-[c:5]>>[C:3]-[C:2](-[C:4])(-[OH;D1;+0:1])-[c:5]
87.4
[{"value": 87.4, "product": "C1=CC(=C(C=C1F)F)C(CN2C=NC=N2)(CN3C=NC=N3)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.3, "product": "C1=CC(=C(C=C1F)F)C(CN2C=NC=N2)(CN3C=NC=N3)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A mixture of 7.5 g (0.02 mol) of 2-(2,4-difluorophenyl)-1,3-bis(1,2,4-triazole-1-yl)-2-(trimethylsilyloxy)propane, 40 ml of methanol, 3 ml of water and 0.1 g of sodium hydroxide was stirred at room temperature for 1 h. After adding 300 ml of water the solution was concentrated to a volume of 50 ml with vacuum distillat...
10.6084/m9.figshare.5104873.v1
null
Silyl protective group
Tertiary alcohol
null
null
c1nc[nH]n1.c1nc[nH]n1.c1ccccc1
Other
O
null
1
C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F>O>OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-480e5f12a0f94e4fa19353d5e0dfbe3c
C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F>>OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
FC1=C(C=CC(=C1)F)C(CN1N=CN=C1)(CN1N=CN=C1)O[Si](C)(C)C.CO.[OH-].[Na+]>>C1=CC(=C(C=C1F)F)C(CN2C=NC=N2)(CN3C=NC=N3)O
C[Si](C)(C)[O:1][C:2]([CH2:3][n:4]1[cH:5][n:6][cH:7][n:8]1)([CH2:9][n:10]1[cH:11][n:12][cH:13][n:14]1)[c:15]1[cH:16][cH:17][c:18]([F:19])[cH:20][c:21]1[F:22]>>[OH:1][C:2]([CH2:3][n:4]1[cH:5][n:6][cH:7][n:8]1)([CH2:9][n:10]1[cH:11][n:12][cH:13][n:14]1)[c:15]1[cH:16][cH:17][c:18]([F:19])[cH:20][c:21]1[F:22]
C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
null
null
O
Deprotection
Alcohol deprotection from silyl ethers
6d1f3bf0e00171fd9431270b3a5c35c615a5f2d97feae7c0a7b6dc8ba859d8aa
bf9cbf8f6c3a5d5e13b674dc7a2b872a6c60a00401e068847221a255cbca9558
c1ccc(C(Cn2cncn2)Cn2cncn2)cc1
C-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])(-[C:4])-[c:5]>>[C:3]-[C:2](-[C:4])(-[OH;D1;+0:1])-[c:5]
89
[{"value": 87.4, "product": "C1=CC(=C(C=C1F)F)C(CN2C=NC=N2)(CN3C=NC=N3)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.0, "product": "C1=CC(=C(C=C1F)F)C(CN2C=NC=N2)(CN3C=NC=N3)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A mixture of 7.5 g (0.02 mol) of 2-(2,4-difluorophenyl)-1,3-bis(1,2,4-triazole-1-yl)-2-(trimethylsilyloxy)propane, 40 ml of methanol, 3 ml of water and 0.1 g of sodium hydroxide was stirred at room temperature for 1 h. After adding 300 ml of water the solution was concentrated to a volume of 50 ml with vacuum distillat...
10.6084/m9.figshare.5104873.v1
null
Silyl protective group
Tertiary alcohol
null
null
c1nc[nH]n1.c1nc[nH]n1.c1ccccc1
Other
O
null
1
C[Si](C)(C)OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F>O>OC(Cn1cncn1)(Cn1cncn1)c1ccc(F)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4c3d7276b6f746199ab6434788921770
CCCC(C(=O)O)=C1SC[C@H]2[C@@H]1N(Cc1ccccc1)C(=O)N2Cc1ccccc1>>CCCC(C(=O)O)C1SC[C@H]2[C@@H]1N(Cc1ccccc1)C(=O)N2Cc1ccccc1
O=C1N([C@H]2[C@@H](N1CC1=CC=CC=C1)CSC2=C(C(=O)O)CCC)CC2=CC=CC=C2.[OH-].[Na+].[H][H]>>O=C1N([C@H]2[C@@H](N1CC1=CC=CC=C1)CSC2C(C(=O)O)CCC)CC2=CC=CC=C2
[CH3:1][CH2:2][CH2:3][C:4]([C:5](=[O:6])[OH:7])=[C:8]1[S:9][CH2:10][C@H:11]2[C@@H:12]1[N:13]([CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1)[C:21](=[O:22])[N:23]2[CH2:24][c:25]1[cH:26][cH:27][cH:28][cH:29][cH:30]1>>[CH3:1][CH2:2][CH2:3][CH:4]([C:5](=[O:6])[OH:7])[CH:8]1[S:9][CH2:10][C@H:11]2[C@@H:12]1[N:13]([CH2:1...
CCCC(C(=O)O)=C1SC[C@H]2[C@@H]1N(Cc1ccccc1)C(=O)N2Cc1ccccc1
CCCC(C(=O)O)C1SC[C@H]2[C@@H]1N(Cc1ccccc1)C(=O)N2Cc1ccccc1
null
[Pd]
O
Reduction
Hydrogenation (double to single)
56117d34fca93ce7bdb006f432bbbbc4f9d0278f718c367e0efaeae3929f8de9
229264280d760663074461f898bce2a68d1dd7a993ad956085f2c6522e0edd11
O=C1N(Cc2ccccc2)[C@@H]2CSC[C@@H]2N1Cc1ccccc1
[C:1]-[#7:2]1-[C:3]2-[C:4](-[#7:5]-[C:6]-1=[O;D1;H0:7])-[C:8]-[#16:9]-[C;H0;D3;+0:10]-2=[C;H0;D3;+0:11](-[C:12]-[C:13])-[C:14](=[O;D1;H0:15])-[O;D1;H1:16]>>[C:1]-[#7:2]1-[C:3]2-[C:4](-[#7:5]-[C:6]-1=[O;D1;H0:7])-[C:8]-[#16:9]-[CH;D3;+0:10]-2-[CH;D3;+0:11](-[C:12]-[C:13])-[C:14](=[O;D1;H0:15])-[O;D1;H1:16]
95.5
[{"value": 95.5, "product": "O=C1N([C@H]2[C@@H](N1CC1=CC=CC=C1)CSC2C(C(=O)O)CCC)CC2=CC=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.5, "product": "O=C1N([C@H]2[C@@H](N1CC1=CC=CC=C1)CSC2C(C(=O)O)CCC)CC2=CC=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
100 g of (3aS, 6aR)hexahydro2-oxo-1,3-dibenzylthieno[3,4-d]imidazol-4-ylidenepentanoic acid (formula I) are dissolved in 340 ml of water at 40° C., where the pH is set to 8.7 using aqueous sodium hydroxide solution. 25% by weight of 5% Pd/C are added to the solution. The mixture is subsequently hydrogenated at an H2 pr...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Monosulfide
C1[NH][C@H]2CSC[C@H]2[NH]1
C1[NH][C@H]2CSC[C@H]2[NH]1
c1ccccc1.C1[NH][C@H]2CSC[C@H]2[NH]1.c1ccccc1
null
[Pd].O
null
null
CCCC(C(=O)O)=C1SC[C@H]2[C@@H]1N(Cc1ccccc1)C(=O)N2Cc1ccccc1>[Pd].O>CCCC(C(=O)O)C1SC[C@H]2[C@@H]1N(Cc1ccccc1)C(=O)N2Cc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7c8877349ecd41a09bb37cf0c4de17f1
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl>>N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl
C([O-])(O)=O.[Na+].ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NN=C(C#N)CC#N.[C-]#N.[Na+].O>>ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NNC(C#N)CC#N
[N:1]#[C:2][CH2:3][C:4]([C:5]#[N:6])=[N:7][NH:8][c:9]1[c:10]([Cl:11])[cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][c:19]1[Cl:20]>>[N:1]#[C:2][CH2:3][CH:4]([C:5]#[N:6])[NH:7][NH:8][c:9]1[c:10]([Cl:11])[cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][c:19]1[Cl:20]
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl
N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl
null
null
C(C)(=O)O
Reduction
OtherReaction
5407f493a1ccf8dd5d07d54ae38e6a10270ea7ce5de5a6b7714c1deac546b85e
e98fc89254846fe35f9c53f13405831fb1e12dbc5358868ae840bffa7ffc2275
c1ccccc1
[N;D1;H0:1]#[C:2]-[C:3]-[C;H0;D3;+0:4](-[C:5]#[N;D1;H0:6])=[N;H0;D2;+0:7]-[#7:8]-[c:9]>>[N;D1;H0:1]#[C:2]-[C:3]-[CH;D3;+0:4](-[C:5]#[N;D1;H0:6])-[NH;D2;+0:7]-[#7:8]-[c:9]
40
[{"value": 40.0, "product": "ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NNC(C#N)CC#N", "details": "PERCENTYIELD", "is_desired": false}]
null
null
40
HOUR
2-(2,6-Dichloro-4-trifluoromethylphenylhydrazono) succinonitrile (0.296 g, 1 mmol), sodium cyanide (0.196 g, 4 equivalents), water (1 ml) and acetic acid (5 ml) were added successively to a sealed tube. After reacting for 40 hours at 20° C., the mixture was added to saturated sodium bicarbonate solution, extracted (dic...
10.6084/m9.figshare.5104873.v1
null
Hydrazone
Hydrazine
null
null
c1ccccc1
null
C(C)(=O)O
null
40
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl>C(C)(=O)O>N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-51889edae8a3452c876a139b2f003a44
N#CCCNNc1c(Cl)cc(C(F)(F)F)cc1Cl>>N#CCC=NNc1c(Cl)cc(C(F)(F)F)cc1Cl.N#CCCN=Nc1c(Cl)cc(C(F)(F)F)cc1Cl
ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NNCCC#N>>ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NN=CCC#N.ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)N=NCCC#N
[N:1]#[C:2][CH2:3][CH2:4][NH:5][NH:6][c:7]1[c:8]([Cl:9])[cH:10][c:11]([C:12]([F:13])([F:15])[F:33])[cH:16][c:17]1[Cl:18]>>[N:1]#[C:2][CH2:3][CH:4]=[N:5][NH:6][c:7]1[c:8]([Cl:9])[cH:10][c:11]([C:12]([F:13])([F:14])[F:15])[cH:16][c:17]1[Cl:18].[N:19]#[C:20][CH2:21][CH2:22][N:23]=[N:24][c:25]1[c:26]([Cl:27])[cH:28][c:29](...
N#CCCNNc1c(Cl)cc(C(F)(F)F)cc1Cl
N#CCC=NNc1c(Cl)cc(C(F)(F)F)cc1Cl.N#CCCN=Nc1c(Cl)cc(C(F)(F)F)cc1Cl
null
null
ClC1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
ed8aad37eaaa5ec92e31575847810e2cf3e9924d0be11e1846f6a8b90af167b0
1dcb17eb3b544a058222c99dcf2a97e724801be2ed0154d7db881d9d0bbe9100
c1ccccc1.c1ccccc1
[F;D1;H0:1]-[C;H0;D4;+0:2](-[F;D1;H0:3])(-[F;H0;D1;+0:4])-[c:5](:[c:6]):[c:7].[N;D1;H0:8]#[C:9]-[C:10]-[CH2;D2;+0:11]-[NH;D2;+0:12]-[#7:13]-[c:14]>>[F;D1;H0:1]-[C;H0;D4;+0:2](-[F;D1;H0:15])(-[F;D1;H0:3])-[c:5](:[c:6]):[c:7].[N;D1;H0:8]#[C:9]-[C:10]-[CH;D2;+0:11]=[N;H0;D2;+0:12]-[#7:13]-[c:14].[F;D1;H0:16]-[C:17](-[F;D1...
null
[]
65
CELSIUS
null
null
Cupric chloride (0.673 g, 2.5 equivalents) was added in one portion to a solution of 3-(2,6-dichloro-4-trifluoromethylphenylhydrazino)propionitrile (0.591 g, 2 mmol) in chlorobenzene, and the mixture heated at 65° C. for 50 minutes. The reaction was judged to be complete and was cooled, washed (water), dried (magnesium...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Trifluoro group
Hydrazone.Trifluoro group.Trifluoro group.Aromatic halide.Aromatic halide.Diazene.Nitrile
null
c1ccccc1
c1ccccc1.c1ccccc1
Other
ClC1=CC=CC=C1
65
null
N#CCCNNc1c(Cl)cc(C(F)(F)F)cc1Cl>ClC1=CC=CC=C1>N#CCC=NNc1c(Cl)cc(C(F)(F)F)cc1Cl.N#CCCN=Nc1c(Cl)cc(C(F)(F)F)cc1Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-baf1448600b24f08910c52ab2c44d07b
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl>>N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl
C([O-])(O)=O.[Na+].ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NN=C(C#N)CC#N.[C-]#N.[Na+].O>>ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NNC(C#N)CC#N
[N:1]#[C:2][CH2:3][C:4]([C:5]#[N:6])=[N:7][NH:8][c:9]1[c:10]([Cl:11])[cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][c:19]1[Cl:20]>>[N:1]#[C:2][CH2:3][CH:4]([C:5]#[N:6])[NH:7][NH:8][c:9]1[c:10]([Cl:11])[cH:12][c:13]([C:14]([F:15])([F:16])[F:17])[cH:18][c:19]1[Cl:20]
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl
N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl
null
null
C(C)(=O)O
Reduction
OtherReaction
5407f493a1ccf8dd5d07d54ae38e6a10270ea7ce5de5a6b7714c1deac546b85e
e98fc89254846fe35f9c53f13405831fb1e12dbc5358868ae840bffa7ffc2275
c1ccccc1
[N;D1;H0:1]#[C:2]-[C:3]-[C;H0;D3;+0:4](-[C:5]#[N;D1;H0:6])=[N;H0;D2;+0:7]-[#7:8]-[c:9]>>[N;D1;H0:1]#[C:2]-[C:3]-[CH;D3;+0:4](-[C:5]#[N;D1;H0:6])-[NH;D2;+0:7]-[#7:8]-[c:9]
40
[{"value": 40.0, "product": "ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NNC(C#N)CC#N", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-(2,6-Dichloro-4-trifluoromethylphenylhydrazono) succinonitrile (0.296 g, 1 mmol), sodium cyanide (0.196 g, 4 equivalents), water (1 ml) and acetic acid (5 ml) were added successively to a tube, which was sealed and reacted at 20° C. for 40 hours. The mixture was added to saturated sodium bicarbonate solution, extract...
10.6084/m9.figshare.5104873.v1
null
Hydrazone
Hydrazine
null
null
c1ccccc1
null
C(C)(=O)O
null
null
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl>C(C)(=O)O>N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-67a56ca062ed49e28806d7fa817ae8e6
N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl>>N#Cc1cc(N)n(-c2c(Cl)cc(C(F)(F)F)cc2Cl)n1
ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NNC(C#N)CC#N>>NC1=CC(=NN1C1=C(C=C(C=C1Cl)C(F)(F)F)Cl)C#N
[N:1]#[C:2][CH:3]([CH2:4][C:5]#[N:6])[NH:20][NH:7][c:8]1[c:9]([Cl:10])[cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17][c:18]1[Cl:19]>>[N:1]#[C:2][c:3]1[cH:4][c:5]([NH2:6])[n:7](-[c:8]2[c:9]([Cl:10])[cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17][c:18]2[Cl:19])[n:20]1
N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl
N#Cc1cc(N)n(-c2c(Cl)cc(C(F)(F)F)cc2Cl)n1
null
null
ClC1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
b468450357c340324b27ad221956f278e770d5b03898c74e823c1dcc5fe3860a
5092d92c44a94ca732d9d3d84dd7211867770f6f2163d1b48afa6352f7be4e62
c1ccc(-n2cccn2)cc1
[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[NH;D2;+0:5]-[NH;D2;+0:6]-[CH;D3;+0:7](-[C:8]#[N;D1;H0:9])-[CH2;D2;+0:10]-[C;H0;D2;+0:11]#[N;H0;D1;+0:12]):[c:13](-[Cl;D1;H0:14]):[c:15]>>[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[n;H0;D3;+0:5]1:[n;H0;D2;+0:6]:[c;H0;D3;+0:7](-[C:8]#[N;D1;H0:9]):[cH;D2;+0:10]:[c;H0;D3;+0:11]:...
null
[]
null
null
null
null
A mixture of 2-(2,6-dichloro-4-trifluoromethylphenylhydrazino)succinonitrile (0.323 g) and cupric chloride (0.175 g) was heated in chlorobenzene at 60° C. for 6 hours. After filtration and evaporation, the title compound and 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole were obtained as a 7:1 mixture...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Nitrile
Primary amine
null
c1cc[nH]n1
c1cc[nH]n1.c1ccccc1
null
ClC1=CC=CC=C1
null
null
N#CCC(C#N)NNc1c(Cl)cc(C(F)(F)F)cc1Cl>ClC1=CC=CC=C1>N#Cc1cc(N)n(-c2c(Cl)cc(C(F)(F)F)cc2Cl)n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cb61453604094862921209455778ae62
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl>>N#Cc1cc(N)n(-c2c(Cl)cc(C(F)(F)F)cc2Cl)n1
N.N.ClC1=C(C(=CC(=C1)C(F)(F)F)Cl)NN=C(C#N)CC#N>>NC1=CC(=NN1C1=C(C=C(C=C1Cl)C(F)(F)F)Cl)C#N
[N:1]#[C:2][C:3]([CH2:4][C:5]#[N:6])=[N:20][NH:7][c:8]1[c:9]([Cl:10])[cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17][c:18]1[Cl:19]>>[N:1]#[C:2][c:3]1[cH:4][c:5]([NH2:6])[n:7](-[c:8]2[c:9]([Cl:10])[cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17][c:18]2[Cl:19])[n:20]1
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl
N#Cc1cc(N)n(-c2c(Cl)cc(C(F)(F)F)cc2Cl)n1
null
null
O.C(C)O
Aromatic Heterocycle Formation
OtherReaction
cfb4258ae32ca397a65abc21d2ec0f2a8bd6a228b05fd6c19d030e16cc6afe72
b4269a4e7ce3c60f2dfb38f61cd23fe9d4819f05708cbaa9dd0a1418dfe3a6ec
c1ccc(-n2cccn2)cc1
[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[NH;D2;+0:5]-[N;H0;D2;+0:6]=[C;H0;D3;+0:7](-[C:8]#[N;D1;H0:9])-[CH2;D2;+0:10]-[C;H0;D2;+0:11]#[N;H0;D1;+0:12]):[c:13](-[Cl;D1;H0:14]):[c:15]>>[Cl;D1;H0:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[n;H0;D3;+0:5]1:[n;H0;D2;+0:6]:[c;H0;D3;+0:7](-[C:8]#[N;D1;H0:9]):[cH;D2;+0:10]:[c;H0;D3;+0:...
98.7
[{"value": 97.0, "product": "NC1=CC(=NN1C1=C(C=C(C=C1Cl)C(F)(F)F)Cl)C#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.7, "product": "NC1=CC(=NN1C1=C(C=C(C=C1Cl)C(F)(F)F)Cl)C#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
Ammonia (20 microliters of an 8% ammonia solution in water) was added to a mixture of the above 2-(2,6-dichloro-4—trifluoromethylphenylhydrazono)-succinonitrile (0.077 g) in ethanol (1 ml) and water (0.2 ml) at 0° C. After 10 minutes, the mixture was extracted (dichloromethane) and evaporated to give 5amino-3-cyano-1-(...
10.6084/m9.figshare.5104873.v1
null
Hydrazone.Nitrile
Primary amine
null
c1cc[nH]n1
c1cc[nH]n1.c1ccccc1
null
O.C(C)O
null
0.166667
N#CCC(C#N)=NNc1c(Cl)cc(C(F)(F)F)cc1Cl>O.C(C)O>N#Cc1cc(N)n(-c2c(Cl)cc(C(F)(F)F)cc2Cl)n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1e075a27cd2c4e05b06018d53454909d
ClP(Cl)c1csc2ccccc12>>Pc1csc2ccccc12
[H-].[H-].[H-].[H-].[Li+].[Al+3].C1CCOC1.ClP(C1=CSC2=C1C=CC=C2)Cl.[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+]>>PC1=CSC2=C1C=CC=C2
Cl[P:1](Cl)[c:2]1[cH:3][s:4][c:5]2[cH:6][cH:7][cH:8][cH:9][c:10]12>>[PH2:1][c:2]1[cH:3][s:4][c:5]2[cH:6][cH:7][cH:8][cH:9][c:10]12
ClP(Cl)c1csc2ccccc12
Pc1csc2ccccc12
null
null
C(C)OCC.CCOCC
Functional Group Interconversion
OtherReaction
42af6cdfb86a130c92365e01a31b50705eea7bdf12f67dc370bf24402f7ceedc
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
c1ccc2sccc2c1
Cl-[P;H0;D3;+0:1](-Cl)-[c:2]1:[c:3]:[c:4]:[#16;a:5]:[c:6]:1>>[PH2;D1;+0:1]-[c:2]1:[c:3]:[c:4]:[#16;a:5]:[c:6]:1
null
[]
null
null
null
null
Under a nitrogen atmosphere a three necked 1 L flask was charged with diethyl ether (200 ml) and a solution of LiAlH4 in THF (58 mL of 1 N solution, 58 mmol). A solution of 3-bis(chloro)phosphino benzo[d]thiophene (18.24 g, 77.6 mmol) in ether (ca. 40 mL) was added dropwise over ca. 30 minutes. An exothermic reaction t...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccc2sccc2c1
Other
C(C)OCC.CCOCC
null
null
ClP(Cl)c1csc2ccccc12>C(C)OCC.CCOCC>Pc1csc2ccccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d2db2c76d76647879b5756d327a4ecdc
CCCCCCC.CCNCC.C[C@H](O)CC[C@H](C)O.Pc1sc2ccccc2c1P.[Li][CH2]CCC>>C[C@@H]1CC[C@@H](C)P1c1sc2ccccc2c1P1[C@H](C)CC[C@H]1C
[Li]N(CC)CC.C[C@@H](CC[C@H](C)O)O.PC1=C(C2=C(S1)C=CC=C2)P.[Li]N(CC)CC.[Li]N(CC)CC.N(CC)CC.[Li]CCCC.CCCCCCC>>C[C@H]1P([C@@H](CC1)C)C1=C(C2=C(S1)C=CC=C2)P2[C@@H](CC[C@H]2C)C
CCCCCC[CH3:23].CCNC[CH3:19].O[C@@H:2]([CH3:1])[CH2:3][CH2:4][C@@H:5](O)[CH3:6].[PH2:7][c:8]1[s:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1[PH2:17].[Li][CH2:18][CH2:20][CH2:21][CH3:22]>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][C@@H:5]([CH3:6])[P:7]1[c:8]1[s:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1[P:17]1[C@H:18...
CCCCCCC.CCNCC.C[C@H](O)CC[C@H](C)O.Pc1sc2ccccc2c1P.[Li][CH2]CCC
C[C@@H]1CC[C@@H](C)P1c1sc2ccccc2c1P1[C@H](C)CC[C@H]1C
null
null
C1CCOC1.O.C(C)OCC
C-C Coupling
OtherReaction
c862e309cff870a4a702548206f63b2de9275a484440e37597fb69ad6a3b9f8f
6fa71b35a61c94f6fc706668cc5e5744bf730f33856b3eadbeabf253252d447a
c1ccc2c(P3CCCC3)c(P3CCCC3)sc2c1
C-C-C-C-C-C-[CH3;D1;+0:1].C-C-N-C-[CH3;D1;+0:2].O-[C@@H;D3;+0:3](-[C;D1;H3:4])-[C:5]-[C:6]-[C@@H;D3;+0:7](-O)-[C;D1;H3:8].[CH3;D1;+0:9]-[C:10]-[C:11]-[CH2;D2;+0:12]-[Li].[PH2;D1;+0:13]-[c:14]1:[c:15]:[c:16]:[#16;a:17]:[c:18]:1-[PH2;D1;+0:19]>>[C;D1;H3:4]-[C@@H;D3;+0:3]1-[C:5]-[C:6]-[C@@H;D3;+0:7](-[C;D1;H3:8])-[P;H0;D3...
53
[{"value": 53.0, "product": "C[C@H]1P([C@@H](CC1)C)C1=C(C2=C(S1)C=CC=C2)P2[C@@H](CC[C@H]2C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
Under argon, a degassed solution of 1.98 g (10 mmol) 2,3-bisphosphinobenzo[b]thiophene in 30 ml THF is treated with 5.5 ml (11 mmol) of a 2N solution of LiNEt2 (freshly prepared from Et2NH and 2.7 M n-BuLi/heptane) in THF. The resulting red solution is added to a degassed solution of the cyclic sulfate derived from (2S...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Secondary alcohol.Secondary amine.Alkyl lithium
null
null
C1CC[P]C1.C1CC[P]C1
C1CC[P]C1.c1ccc2sccc2c1.C1CC[P]C1
HO-.Li
C1CCOC1.O.C(C)OCC
null
2
CCCCCCC.CCNCC.C[C@H](O)CC[C@H](C)O.Pc1sc2ccccc2c1P.[Li][CH2]CCC>C1CCOC1.O.C(C)OCC>C[C@@H]1CC[C@@H](C)P1c1sc2ccccc2c1P1[C@H](C)CC[C@H]1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c9e588b9fb2e4e3d96164ee2aa8ac6ed
CC[C@H](O)CC[C@@H](O)CC.Pc1sc2ccccc2c1P>>CC[C@@H]1CC[C@@H](CC)P1c1sc2ccccc2c1P1[C@H](CC)CC[C@H]1CC
CC[C@@H](CC[C@H](CC)O)O.PC1=C(C2=C(S1)C=CC=C2)P>>C(C)[C@H]1P([C@@H](CC1)CC)C1=C(C2=C(S1)C=CC=C2)P2[C@@H](CC[C@H]2CC)CC
O[C@@H:3]([CH2:2][CH3:1])[CH2:4][CH2:23][C@@H:20](O)[CH2:21][CH3:22].[PH2:9][c:10]1[s:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[c:18]1[PH2:19]>>[CH3:1][CH2:2][C@@H:3]1[CH2:4][CH2:5][C@@H:6]([CH2:7][CH3:8])[P:9]1[c:10]1[s:11][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]2[c:18]1[P:19]1[C@H:20]([CH2:21][CH3:22])[CH2:23][C...
CC[C@H](O)CC[C@@H](O)CC.Pc1sc2ccccc2c1P
CC[C@@H]1CC[C@@H](CC)P1c1sc2ccccc2c1P1[C@H](CC)CC[C@H]1CC
null
null
null
C-C Coupling
OtherReaction
945ea16d13907ab8ecd95e7bb3af650bedd656b551e6cefce2341d4ad5401cba
d31b1403224a2056c6fea4b48c2e4a296abf1f6d3f650f72956bbe0c3270c86f
c1ccc2c(P3CCCC3)c(P3CCCC3)sc2c1
O-[C@@H;D3;+0:1](-[C:2]-[C;D1;H3:3])-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[C@@H;D3;+0:6](-O)-[C:7]-[C;D1;H3:8].[PH2;D1;+0:9]-[c:10]1:[c:11]:[c:12]:[#16;a:13]:[c:14]:1-[PH2;D1;+0:15]>>[C:16]-[C:17]1-[C:18]-[CH2;D2;+0:4]-[C@@H;D3;+0:1](-[C:2]-[C;D1;H3:3])-[P;H0;D3;+0:9]-1-[c:10]1:[c:11]:[c:12]:[#16;a:13]:[c:14]:1-[P;H0;D3;+0:15]1...
48
[{"value": 48.0, "product": "C(C)[C@H]1P([C@@H](CC1)CC)C1=C(C2=C(S1)C=CC=C2)P2[C@@H](CC[C@H]2CC)CC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
In analogy to Example 11, the cyclic sulfate derived from (3S,6S)-3,6-octanediol is reacted with 2,3-bisphosphinobenzo[b]thiophene to give the title compound in 48% yield. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Secondary alcohol
null
null
C1CC[P]C1.C1CC[P]C1
C1CC[P]C1.c1ccc2sccc2c1.C1CC[P]C1
null
null
null
null
CC[C@H](O)CC[C@@H](O)CC.Pc1sc2ccccc2c1P>>CC[C@@H]1CC[C@@H](CC)P1c1sc2ccccc2c1P1[C@H](CC)CC[C@H]1CC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9f2ddd4ffff34606b2cc625dff14a9fc
CN1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>>CN1CCN(c2ccc(N=C=S)cc2)CC1
C(=S)(N1C=NC=C1)N1C=NC=C1.CN1CCN(CC1)C1=CC=C(C=C1)N>>N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH2:10])[cH:13][cH:14]2)[CH2:15][CH2:16]1.c1cn([C:11](n2ccnc2)=[S:12])cn1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:12])[cH:13][cH:14]2)[CH2:15][CH2:16]1
CN1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1
CN1CCN(c2ccc(N=C=S)cc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCNCC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
83
[{"value": 83.0, "product": "N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C", "details": "PERCENTYIELD", "is_desired": false}]
-15
CELSIUS
1
HOUR
A mixture of thiocarbonyldiimidazole (4.46 g, 25.0 mmol) (Aldrich) and N,N-dimethylformamide (20 mL) was cooled to about −15° C. and a solution of 4-(4-methyl-1-piperazinyl)benzenamine (prepared according to the procedure of Chong, W. K. et al. WO9921845; 4.78 g, 25.0 mmol) was added over a period of 30 min. The coolin...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
C1C[NH]CC[NH]1.c1ccccc1
Other
CN(C=O)C
-15
1
CN1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>CN(C=O)C>CN1CCN(c2ccc(N=C=S)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7fc712df9bea40238aa90ddb61a7176d
CN1CCNCC1.O=[N+]([O-])c1ccc(F)c(F)c1>>CN1CCN(c2ccc([N+](=O)[O-])cc2F)CC1
FC=1C=C(C=CC1F)[N+](=O)[O-].CN1CCNCC1>>FC1=C(C=CC(=C1)[N+](=O)[O-])N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][NH:5][CH2:16][CH2:17]1.F[c:6]1[cH:7][cH:8][c:9]([N+:10](=[O:11])[O-:12])[cH:13][c:14]1[F:15]>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N+:10](=[O:11])[O-:12])[cH:13][c:14]2[F:15])[CH2:16][CH2:17]1
CN1CCNCC1.O=[N+]([O-])c1ccc(F)c(F)c1
CN1CCN(c2ccc([N+](=O)[O-])cc2F)CC1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation secondary amine
d687b31bdda9f407fdde6ca57e67eee0681e173646c617afef7770c56d05bab9
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc(N2CCNCC2)cc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[F;D1;H0:5]):[c:6].[#7:7]1-[C:8]-[C:9]-[NH;D2;+0:10]-[C:11]-[C:12]-1>>[F;D1;H0:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[N;H0;D3;+0:10]1-[C:9]-[C:8]-[#7:7]-[C:12]-[C:11]-1):[c:2]:[c:3]
97
[{"value": 97.0, "product": "FC1=C(C=CC(=C1)[N+](=O)[O-])N1CCN(CC1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.0, "product": "FC1=C(C=CC(=C1)[N+](=O)[O-])N1CCN(CC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of 3,4-difluoronitrobenzene (12.00 g, 75.4 mmol) (Aldrich) and N-methylpiperazine (18.89 g, 188.6 mmol) in acetonitrile (150 mL) was heated at reflux for 3 h. The reaction mixture was allowed to stand overnight at room temperature, then the solvent was evaporated under reduced pressure and the residue was pa...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1C[NH]CCN1.c1ccccc1
C1C[NH]CC[NH]1.c1ccccc1
C1C[NH]CC[NH]1.c1ccccc1
HF
C(C)#N
null
8
CN1CCNCC1.O=[N+]([O-])c1ccc(F)c(F)c1>C(C)#N>CN1CCN(c2ccc([N+](=O)[O-])cc2F)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-864b47b038fb440aa3f650a6dea2c1e2
CN1CCN(c2ccc([N+](=O)[O-])cc2F)CC1>>CN1CCN(c2ccc(N)cc2F)CC1
FC1=C(C=CC(=C1)[N+](=O)[O-])N1CCN(CC1)C>>FC=1C=C(C=CC1N1CCN(CC1)C)N
O=[N+:10]([O-])[c:9]1[cH:8][cH:7][c:6]([N:5]2[CH2:4][CH2:3][N:2]([CH3:1])[CH2:15][CH2:14]2)[c:12]([F:13])[cH:11]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH2:10])[cH:11][c:12]2[F:13])[CH2:14][CH2:15]1
CN1CCN(c2ccc([N+](=O)[O-])cc2F)CC1
CN1CCN(c2ccc(N)cc2F)CC1
null
[Pd]
C(C)(=O)OCC.C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(N2CCNCC2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
93
[{"value": 93.0, "product": "FC=1C=C(C=CC1N1CCN(CC1)C)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.6, "product": "FC=1C=C(C=CC1N1CCN(CC1)C)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 1-(2-fluoro-4-nitrophenyl)-4-methylpiperazine (5.00 g, 20.9 mmol) (from Step A above) and 10% palladium-on-carbon (0.20 g, 0.2 mmol) in ethyl acetate (100 mL) and ethanol (50 mL) was hydrogenated at 50 psi in a Parr shaker for 4 h. The mixture was filtered through Celite™. The Celite™ was washed with ethy...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
C1C[NH]CC[NH]1.c1ccccc1
Other
[Pd].C(C)(=O)OCC.C(C)O
null
null
CN1CCN(c2ccc([N+](=O)[O-])cc2F)CC1>[Pd].C(C)(=O)OCC.C(C)O>CN1CCN(c2ccc(N)cc2F)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8e88da186bb64330afe884ecd3c3eb32
CN1CCN(c2ccc(N)cc2F)CC1.S=C(c1ncc[nH]1)c1ncc[nH]1>>CN1CCN(c2ccc(N=C=S)cc2F)CC1
FC=1C=C(C=CC1N1CCN(CC1)C)N.C(=S)(C=1NC=CN1)C=1NC=CN1>>FC1=C(C=CC(=C1)N=C=S)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH2:10])[cH:13][c:14]2[F:15])[CH2:16][CH2:17]1.c1c[nH]c([C:11](c2ncc[nH]2)=[S:12])n1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:12])[cH:13][c:14]2[F:15])[CH2:16][CH2:17]1
CN1CCN(c2ccc(N)cc2F)CC1.S=C(c1ncc[nH]1)c1ncc[nH]1
CN1CCN(c2ccc(N=C=S)cc2F)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCNCC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-c1:[nH]:c:c:n:1)-c1:[nH]:c:c:n:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
8
HOUR
Thiocarbonyl diimidazole (3.00 g, 3.53 mmol) (Aldrich) was dissolved in N,N-dimethylformamide (10 mL) and the solution was cooled to −10° C. (ice/acetone bath). A solution of 3-fluoro-4-(4-methyl-1-piperazinyl) benzenamine (2.26 g, 10.8 mmol) (from Step B above) in N,N-dimethylformamide (30 mL) was added over a period ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
C1C[NH]CC[NH]1.c1ccccc1
Other
CN(C=O)C
null
8
CN1CCN(c2ccc(N)cc2F)CC1.S=C(c1ncc[nH]1)c1ncc[nH]1>CN(C=O)C>CN1CCN(c2ccc(N=C=S)cc2F)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9f2a80a91dcc4887a781077f3e4406f3
CC(C)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>>CC(C)N1CCN(c2ccc(N=C=S)cc2)CC1
CC(C)N1CCN(CC1)C1=CC=C(C=C1)N.C(=S)(N1C=NC=C1)N1C=NC=C1>>N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(C)C
[CH3:1][CH:2]([CH3:3])[N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([NH2:12])[cH:15][cH:16]2)[CH2:17][CH2:18]1.c1cn([C:13](n2ccnc2)=[S:14])cn1>>[CH3:1][CH:2]([CH3:3])[N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([N:12]=[C:13]=[S:14])[cH:15][cH:16]2)[CH2:17][CH2:18]1
CC(C)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1
CC(C)N1CCN(c2ccc(N=C=S)cc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCNCC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
101.3
[{"value": 101.3, "product": "N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-15
CELSIUS
20
MINUTE
A solution of 4-[4-(1-methylethyl)-1-piperazinyl]benzenamine (1.6 g,˜6.8 mmol) (from Step B above) in N,N-dimethylformamide (25 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (1.4 g, 7.7 mmol) (Aldrich) in N,N-dimethylformamide (30 mL). After the addition was complete, the ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
C1C[NH]CC[NH]1.c1ccccc1
Other
CN(C=O)C
-15
0.333333
CC(C)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>CN(C=O)C>CC(C)N1CCN(c2ccc(N=C=S)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-994cbfeb630d41b6b2862208213baf98
CC(=O)Cl.O=[N+]([O-])c1ccc(N2CCNCC2)cc1>>CC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1
C([O-])([O-])=O.[K+].[K+].C(C)(=O)Cl.[N+](=O)([O-])C1=CC=C(C=C1)N1CCNCC1.C([O-])([O-])=O.[K+].[K+].C(C)(=O)Cl>>C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)[N+](=O)[O-]
Cl[C:2]([CH3:1])=[O:3].[NH:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([N+:12](=[O:13])[O-:14])[cH:15][cH:16]2)[CH2:17][CH2:18]1>>[CH3:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([N+:12](=[O:13])[O-:14])[cH:15][cH:16]2)[CH2:17][CH2:18]1
CC(=O)Cl.O=[N+]([O-])c1ccc(N2CCNCC2)cc1
CC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1
null
null
ClCCl
Acylation
N-alkylation of secondary amines with alkyl halides
6dd420fad17fb719b6bd840e8952a8d7b2fb24721f86f8b8f9c697a36eb97ec3
96cb0a2fed10552c5770a45a2d6523b47ac3e38928b4a9c698d8577451182dcd
c1ccc(N2CCNCC2)cc1
Cl-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[#7:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-1>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[#7:4]-[C:9]-[C:8]-1
722.1
[{"value": 72.0, "product": "C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 722.1, "product": "C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Powdered potassium carbonate (276 mg, 2 mmol) and then acetyl chloride (0.14 mL, 2 mmol) were added to a solution of 1-(4-nitrophenyl) piperazine (2.1 g, 1 mmol) (Acros Organics) in dichloromethane (75 mL). The mixture was stirred at room temperature overnight and then further quantities of powdered potassium carbonate...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary amine
Tertiary amide
C1CNCC[NH]1
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1ccccc1
HCl
ClCCl
null
8
CC(=O)Cl.O=[N+]([O-])c1ccc(N2CCNCC2)cc1>ClCCl>CC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c84ff7750f7042e88d7b296e98f6f5f4
CC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1>>CC(=O)N1CCN(c2ccc(N)cc2)CC1
C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)[N+](=O)[O-]>>C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)N
O=[N+:12]([O-])[c:11]1[cH:10][cH:9][c:8]([N:7]2[CH2:6][CH2:5][N:4]([C:2]([CH3:1])=[O:3])[CH2:16][CH2:15]2)[cH:14][cH:13]1>>[CH3:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([NH2:12])[cH:13][cH:14]2)[CH2:15][CH2:16]1
CC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1
CC(=O)N1CCN(c2ccc(N)cc2)CC1
null
[Pd]
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(N2CCNCC2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
63.3
[{"value": 63.0, "product": "C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 63.3, "product": "C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 1-acetyl-4-(4-nitrophenyl)piperazine (1.8 g, 7.2 mmol) (from Step A above) and 10% palladium-on-charcoal in ethanol (50 mL) was hydrogenated at room temperature and atmospheric pressure overnight. The catalyst was filtered off and the filter cake washed thoroughly with ethanol. The mixture was evaporated u...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
C1C[NH]CC[NH]1.c1ccccc1
Other
[Pd].C(C)O
null
null
CC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1>[Pd].C(C)O>CC(=O)N1CCN(c2ccc(N)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-791ac1550fd64af8a5667939b1f90372
CC(=O)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>>CC(=O)N1CCN(c2ccc(N=C=S)cc2)CC1
C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)N.C(=S)(N1C=NC=C1)N1C=NC=C1>>C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)N=C=S
[CH3:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([NH2:12])[cH:15][cH:16]2)[CH2:17][CH2:18]1.c1cn([C:13](n2ccnc2)=[S:14])cn1>>[CH3:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([N:12]=[C:13]=[S:14])[cH:15][cH:16]2)[CH2:17][CH2:18]1
CC(=O)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1
CC(=O)N1CCN(c2ccc(N=C=S)cc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCNCC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
84
[{"value": 84.0, "product": "C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)N=C=S", "details": "PERCENTYIELD", "is_desired": false}, {"value": 83.2, "product": "C(C)(=O)N1CCN(CC1)C1=CC=C(C=C1)N=C=S", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-15
CELSIUS
30
MINUTE
A solution of 1-acetyl-4-(4-aminophenyl)piperazine (1.0 g, 4.6 mmol) (from Step B above) in N,N-dimethylformamide (10 mL) was added dropwise to a cooled (−15° C.) solution of thiocarbonyldiimidazole (855 mg, 4.8 mmol) in N,N-dimethylformamide (10 mL). After the addition was complete, the mixture was stirred at −15° C. ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
C1C[NH]CC[NH]1.c1ccccc1
Other
CN(C=O)C
-15
0.5
CC(=O)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>CN(C=O)C>CC(=O)N1CCN(c2ccc(N=C=S)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-63144ce9652240199f91e9d2e6bc1107
O=[N+]([O-])c1ccc(N2CCN(CCO)CC2)cc1.[N-]=C=S>>OCCN1CCN(c2ccc(N=C=S)cc2)CC1
[N+](=O)([O-])C1=CC=C(C=C1)N1CCN(CC1)CCO.[N-]=C=S>>OCCN1CCN(CC1)C1=CC=C(C=C1)N=C=S
O=[N+]([O-])[c:11]1[cH:10][cH:9][c:8]([N:7]2[CH2:6][CH2:5][N:4]([CH2:3][CH2:2][OH:1])[CH2:18][CH2:17]2)[cH:16][cH:15]1.[N-:12]=[C:13]=[S:14]>>[OH:1][CH2:2][CH2:3][N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([N:12]=[C:13]=[S:14])[cH:15][cH:16]2)[CH2:17][CH2:18]1
O=[N+]([O-])c1ccc(N2CCN(CCO)CC2)cc1.[N-]=C=S
OCCN1CCN(c2ccc(N=C=S)cc2)CC1
null
null
null
Functional Group Interconversion
OtherReaction
c2b664bf7684468a37396b968ac0af317a7e2289f2edcfb8b7ab78ab404e94b4
305b6f3127a1d497f5798d688e7949ef02b1f99b0e5e183d105619e0875515fa
c1ccc(N2CCNCC2)cc1
O=[N+](-[O-])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[N-;H0;D1:6]=[C:7]=[S;D1;H0:8]>>[S;D1;H0:8]=[C:7]=[N;H0;D2;+0:6]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
null
null
This compound was prepared from 4-(4-nitrophenyl)-1-piperazine-ethanol (Bionet Research Ltd.) using the hydrogenation and isothiocyanate-forming reactions used in Example 4. Conditions: See reaction.notes.procedure_details. Workup: forming reactions
10.6084/m9.figshare.5104873.v1
null
Nitro group
Isothiocyanate
c1ccccc1
c1ccccc1
C1C[NH]CC[NH]1.c1ccccc1
Other
null
null
null
O=[N+]([O-])c1ccc(N2CCN(CCO)CC2)cc1.[N-]=C=S>>OCCN1CCN(c2ccc(N=C=S)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-24cd7e80c0804870b102321d8cc9cb2e
CC(C)(C)OC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1>>CC(C)(C)OC(=O)N1CCN(c2ccc(N)cc2)CC1
[N+](=O)([O-])C1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C.[H][H]>>NC1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C
O=[N+:16]([O-])[c:15]1[cH:14][cH:13][c:12]([N:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:20][CH2:19]2)[cH:18][cH:17]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[cH:13][cH:14][c:15]([NH2:16])[cH:17][cH:18]2)[CH2:19][CH2:20]1
CC(C)(C)OC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1
CC(C)(C)OC(=O)N1CCN(c2ccc(N)cc2)CC1
null
[Pd]
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(N2CCNCC2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
99.8
[{"value": 98.0, "product": "NC1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.8, "product": "NC1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-(4-Nitrophenyl)-1-piperazinecarboxylic acid, 1,1-dimethylethyl ester (20 g, 65 mmol) was dissolved in anhydrous ethanol (250 mL) and 10% Pd/C (1.8 g) was added. The mixture was stirred for 1.5 h under 10 psi of hydrogen and filtered through a Celite pad. The pad was washed with ethyl acetate (3×100 mL) and the combin...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
C1C[NH]CC[NH]1.c1ccccc1
Other
[Pd].C(C)O
null
null
CC(C)(C)OC(=O)N1CCN(c2ccc([N+](=O)[O-])cc2)CC1>[Pd].C(C)O>CC(C)(C)OC(=O)N1CCN(c2ccc(N)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-66c9ae911dbb4a32a0ac6929b789a6cc
CC(C)(C)OC(=O)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>>CC(C)(C)OC(=O)N1CCN(c2ccc(N=C=S)cc2)CC1
NC1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C.C(=S)(N1C=NC=C1)N1C=NC=C1>>N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[cH:13][cH:14][c:15]([NH2:16])[cH:19][cH:20]2)[CH2:21][CH2:22]1.c1cn([C:17](n2ccnc2)=[S:18])cn1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[cH:13][cH:14][c:15]([N:16]=[C:17]=[S:18])[cH:19][cH:20]2...
CC(C)(C)OC(=O)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1
CC(C)(C)OC(=O)N1CCN(c2ccc(N=C=S)cc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCNCC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
104.2
[{"value": 94.0, "product": "N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 104.2, "product": "N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A solution of 4-(4-aminophenyl)-1-piperazinecarboxylic acid, 1,1-dimethylethyl ester (15 g, 54.1 mmol) (from Step B above) in N,N-dimethylformamide (120 mL) was added dropwise to a cooled (−15° C.) solution of 1,1′-thiocarbonyldiimidazole (9.66 g, 54.2 mmol) (Aldrich) in N,N-dimethylformamide (40 mL). After the additio...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
C1C[NH]CC[NH]1.c1ccccc1
Other
CN(C=O)C
null
1
CC(C)(C)OC(=O)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>CN(C=O)C>CC(C)(C)OC(=O)N1CCN(c2ccc(N=C=S)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ff4256aaf0c04c6c9ceb8c97dc41cecd
O=C(c1ccc(N2CCCCC2)cc1)C(Br)Br>>O=C(CBr)c1ccc(N2CCCCC2)cc1
C(C)OP(OCC)[O-].C(C)N(CC)CC.BrC(C(=O)C1=CC=C(C=C1)N1CCCCC1)Br>>BrCC(=O)C1=CC=C(C=C1)N1CCCCC1
Br[CH:3]([C:2](=[O:1])[c:5]1[cH:6][cH:7][c:8]([N:9]2[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]2)[cH:15][cH:16]1)[Br:4]>>[O:1]=[C:2]([CH2:3][Br:4])[c:5]1[cH:6][cH:7][c:8]([N:9]2[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]2)[cH:15][cH:16]1
O=C(c1ccc(N2CCCCC2)cc1)C(Br)Br
O=C(CBr)c1ccc(N2CCCCC2)cc1
null
null
O1CCCC1
Functional Group Interconversion
Dehalogenation
77c4006b61feafdadb38a3464a8de1ee490b61d0da0c13bca01b4c6c32c9e17b
6057d7fb75624930c9e41a46967dce14902ce53987bcfcd5587c4c1a79bea4df
c1ccc(N2CCCCC2)cc1
Br-[CH;D3;+0:1](-[Br;D1;H0:2])-[C:3](=[O;D1;H0:4])-[c:5]>>[Br;D1;H0:2]-[CH2;D2;+0:1]-[C:3](=[O;D1;H0:4])-[c:5]
100
[{"value": 100.0, "product": "BrCC(=O)C1=CC=C(C=C1)N1CCCCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 98.2, "product": "BrCC(=O)C1=CC=C(C=C1)N1CCCCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
2,2-Dibromo-1-[4-(1-piperidinyl)phenyl]ethanone (3 g, 8.3 mmol) (from Step A above) was dissolved in tetrahydrofuran (15 mL), and cooled to 0° C. To the resulting solution were added dropwise diethylphosphite (1.13 mL, 8.7 mmol) and triethylamine (1.21 mL, 8.7 mmol) in tetrahydrofuran (7 mL) at 0° C. with stirring. The...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Secondary halide
Primary halide
null
null
c1ccccc1.C1CC[NH]CC1
Br-
O1CCCC1
0
null
O=C(c1ccc(N2CCCCC2)cc1)C(Br)Br>O1CCCC1>O=C(CBr)c1ccc(N2CCCCC2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-73931fa5a60e46348d2c319123fbab8b
CC(=O)c1ccc(N2CCOCC2)cc1.O=C(CBr)c1ccc(N2CCCCC2)cc1>>O=C(CBr)c1ccc(N2CCOCC2)cc1
N1(CCOCC1)C1=CC=C(C=C1)C(C)=O.BrCC(=O)C1=CC=C(C=C1)N1CCCCC1>>BrCC(=O)C1=CC=C(C=C1)N1CCOCC1
CC(=O)c1c[cH:7][c:8]([N:9]2[CH2:10][CH2:11][O:12][CH2:13][CH2:14]2)[cH:15]c1.c1c(N2CCCCC2)c[cH:16][c:5]([C:2](=[O:1])[CH2:3][Br:4])[cH:6]1>>[O:1]=[C:2]([CH2:3][Br:4])[c:5]1[cH:6][cH:7][c:8]([N:9]2[CH2:10][CH2:11][O:12][CH2:13][CH2:14]2)[cH:15][cH:16]1
CC(=O)c1ccc(N2CCOCC2)cc1.O=C(CBr)c1ccc(N2CCCCC2)cc1
O=C(CBr)c1ccc(N2CCOCC2)cc1
null
null
null
Miscellaneous
Bromination
bc6ef9b1f3fe2b0e61b094d3e6aa4b12aede4c936631a3accb5245309189a7bd
592dfb5f38ca3726bb7bcfb5eeb55519b727530a542db3567e54f180d6649952
c1ccc(N2CCOCC2)cc1
C-C(=O)-c1:c:[cH;D2;+0:1]:[c:2](-[#7:3]):[cH;D2;+0:4]:c:1.[C:5]-[C:6](=[O;D1;H0:7])-[c:8]1:[cH;D2;+0:9]:c:c(-N2-C-C-C-C-C-2):c:[cH;D2;+0:10]:1>>[#7:3]-[c:2]1:[cH;D2;+0:1]:[cH;D2;+0:9]:[c:8](-[C:6](-[C:5])=[O;D1;H0:7]):[cH;D2;+0:10]:[cH;D2;+0:4]:1
null
[]
null
null
null
null
This compound was prepared from 1-[4-(4-morpholinyl)phenyl]ethanone (Aldrich) by procedures analogous to those used to prepare 2-bromo-1-[4-(1-piperidinyl)phenyl]ethanone (Example 7). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Tertiary amine
null
c1ccccc1.c1ccccc1.C1CCNCC1
c1ccccc1
c1ccccc1.C1COCC[NH]1
HO-
null
null
null
CC(=O)c1ccc(N2CCOCC2)cc1.O=C(CBr)c1ccc(N2CCCCC2)cc1>>O=C(CBr)c1ccc(N2CCOCC2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f5d11cfe3cd8412daee3285f06654237
BrBr.CC(=O)Nc1ccc(C(C)=O)cc1>>CC(=O)Nc1ccc(C(=O)CBr)cc1
BrBr.C(C)(=O)C1=CC=C(C=C1)NC(C)=O.C(C)(=O)O>>BrCC(=O)C1=CC=C(C=C1)NC(C)=O
Br[Br:12].[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]([C:9](=[O:10])[CH3:11])[cH:13][cH:14]1>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]([C:9](=[O:10])[CH2:11][Br:12])[cH:13][cH:14]1
BrBr.CC(=O)Nc1ccc(C(C)=O)cc1
CC(=O)Nc1ccc(C(=O)CBr)cc1
null
null
C(Cl)(Cl)(Cl)Cl
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccccc1
Br-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]
97.6
[{"value": 97.6, "product": "BrCC(=O)C1=CC=C(C=C1)NC(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of bromine (0.31 mL, 5.9 mmol) in carbon tetrachloride (10 mL) was added to a suspension of N-(4-acetylphenyl)acetamide (1 g, 5.6 mmol) (Lancaster Synthesis) in carbon tetrachloride (20 mL). The reaction mixture was stirred for several hours but TLC indicated only starting material. Acetic acid (10 mL) was a...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccccc1
HBr
C(Cl)(Cl)(Cl)Cl
null
null
BrBr.CC(=O)Nc1ccc(C(C)=O)cc1>C(Cl)(Cl)(Cl)Cl>CC(=O)Nc1ccc(C(=O)CBr)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1467451901b34110b095a0f9bc4d4385
BrBr.CC(=O)c1ccc(O)cc1>>O=C(CBr)c1ccc(O)cc1
CC(=O)C=1C=CC(=CC1)O.BrBr>>BrCC(=O)C1=CC=C(C=C1)O
Br[Br:4].[O:1]=[C:2]([CH3:3])[c:5]1[cH:6][cH:7][c:8]([OH:9])[cH:10][cH:11]1>>[O:1]=[C:2]([CH2:3][Br:4])[c:5]1[cH:6][cH:7][c:8]([OH:9])[cH:10][cH:11]1
BrBr.CC(=O)c1ccc(O)cc1
O=C(CBr)c1ccc(O)cc1
null
null
O1CCOCC1
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccccc1
Br-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]
44
[{"value": 44.0, "product": "BrCC(=O)C1=CC=C(C=C1)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 44.0, "product": "BrCC(=O)C1=CC=C(C=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a solution of 4-hydroxyacetophenone (2.5 g, 18.3 mmol) (Aldrich) in dioxane (10 mL) was added dropwise a solution of bromine (3.22 g, 20.1 mmol) in dioxane (20 mL). After stirring for 10 minutes, the mixture was concentrated in vacuo and the residue was recrystalized from methanol to provide 2-bromo-1-(4-hydroxyphen...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccccc1
HBr
O1CCOCC1
null
0.166667
BrBr.CC(=O)c1ccc(O)cc1>O1CCOCC1>O=C(CBr)c1ccc(O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a2a922a5821941fc85660d7e312d45ad
BrBr.COc1ccc(C(C)=O)cc1F>>COc1ccc(C(=O)CBr)cc1F
FC=1C=C(C=CC1OC)C(C)=O.BrBr>>BrCC(=O)C1=CC(=C(C=C1)OC)F
Br[Br:10].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([C:7](=[O:8])[CH3:9])[cH:11][c:12]1[F:13]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([C:7](=[O:8])[CH2:9][Br:10])[cH:11][c:12]1[F:13]
BrBr.COc1ccc(C(C)=O)cc1F
COc1ccc(C(=O)CBr)cc1F
null
null
O1CCOCC1
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccccc1
Br-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]
63
[{"value": 63.0, "product": "BrCC(=O)C1=CC(=C(C=C1)OC)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.4, "product": "BrCC(=O)C1=CC(=C(C=C1)OC)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a solution of 3′-fluoro-4′-methoxyacetophenone (1 g, 5.9 mmol) (Aldrich) in dioxane (10 mL) was added dropwise a solution of bromine (1.13 g, 7.1 mmol) in dioxane (30 mL). After stirring for 10 minutes, the mixture was concentrated in vacuo and the residue was purified by flash chromatography, with 10:4 hexanes/dich...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccccc1
HBr
O1CCOCC1
null
0.166667
BrBr.COc1ccc(C(C)=O)cc1F>O1CCOCC1>COc1ccc(C(=O)CBr)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b766bbeecace419eaa52b615ff7cd9e8
BrBr.CC(=O)c1cc(F)cc(F)c1>>O=C(CBr)c1cc(F)cc(F)c1
FC=1C=C(C=C(C1)F)C(C)=O.BrBr>>BrCC(=O)C1=CC(=CC(=C1)F)F
Br[Br:4].[O:1]=[C:2]([CH3:3])[c:5]1[cH:6][c:7]([F:8])[cH:9][c:10]([F:11])[cH:12]1>>[O:1]=[C:2]([CH2:3][Br:4])[c:5]1[cH:6][c:7]([F:8])[cH:9][c:10]([F:11])[cH:12]1
BrBr.CC(=O)c1cc(F)cc(F)c1
O=C(CBr)c1cc(F)cc(F)c1
null
null
O1CCOCC1
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccccc1
Br-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]
64.3
[{"value": 64.0, "product": "BrCC(=O)C1=CC(=CC(=C1)F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 64.3, "product": "BrCC(=O)C1=CC(=CC(=C1)F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a solution of 3′,5′-difluoroacetophenone (3 g, 19.2 mmol) (Lancaster Synthesis) in dioxane (30 mL) was added dropwise a solution of bromine (3.67 g, 23 mmol) in dioxane (75 mL). After stirring for 10 minutes, the mixture was concentrated in vacuo and the residue was purified by flash chromatography, with 10:2 hexane...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccccc1
HBr
O1CCOCC1
null
0.166667
BrBr.CC(=O)c1cc(F)cc(F)c1>O1CCOCC1>O=C(CBr)c1cc(F)cc(F)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0384dff13c2340f491f72741cfa3d6a8
CCC(C)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>>CCC(C)N1CCN(c2ccc(N=C=S)cc2)CC1
C(C)(CC)N1CCN(CC1)C1=CC=C(C=C1)N.C(=S)(N1C=NC=C1)N1C=NC=C1>>N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(C)CC
[CH3:1][CH2:2][CH:3]([CH3:4])[N:5]1[CH2:6][CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([NH2:13])[cH:16][cH:17]2)[CH2:18][CH2:19]1.c1cn([C:14](n2ccnc2)=[S:15])cn1>>[CH3:1][CH2:2][CH:3]([CH3:4])[N:5]1[CH2:6][CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([N:13]=[C:14]=[S:15])[cH:16][cH:17]2)[CH2:18][CH2:19]1
CCC(C)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1
CCC(C)N1CCN(c2ccc(N=C=S)cc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCNCC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
87.1
[{"value": 87.0, "product": "N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(C)CC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.1, "product": "N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(C)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-15
CELSIUS
20
MINUTE
A solution of 4-[4-(sec-butyl)-1-piperazinyl]benzenamine (3.5 g, 15 mmol) (from Step B above) in N,N-dimethylformamide (40 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (2.68 g, 15.03 mmol) (Aldrich) in N,N-dimethylformamide (15 mL). After the addition was complete, the mi...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
C1C[NH]CC[NH]1.c1ccccc1
Other
CN(C=O)C
-15
0.333333
CCC(C)N1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>CN(C=O)C>CCC(C)N1CCN(c2ccc(N=C=S)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e01217a216ad48d18573a7662bc91efb
IC1CCCC1.O=[N+]([O-])c1ccc(N2CCNCC2)cc1>>O=[N+]([O-])c1ccc(N2CCN(C3CCCC3)CC2)cc1
[N+](=O)([O-])C1=CC=C(C=C1)N1CCNCC1.C([O-])([O-])=O.[K+].[K+].IC1CCCC1.C1COCCOCCOCCOCCOCCO1>>C1(CCCC1)N1CCN(CC1)C1=CC=C(C=C1)[N+](=O)[O-]
I[CH:12]1[CH2:13][CH2:14][CH2:15][CH2:16]1.[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([N:8]2[CH2:9][CH2:10][NH:11][CH2:17][CH2:18]2)[cH:19][cH:20]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([N:8]2[CH2:9][CH2:10][N:11]([CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16]3)[CH2:17][CH2:18]2)[cH:19][cH:20]1
IC1CCCC1.O=[N+]([O-])c1ccc(N2CCNCC2)cc1
O=[N+]([O-])c1ccc(N2CCN(C3CCCC3)CC2)cc1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
b79569f0a031da0628617165b9a7f776b7e88b89318685d908026782e56a6194
fb63ba09935e18320be03869002f6d5d0f0321fe7dbcd94a5ae956c3effd182d
c1ccc(N2CCN(C3CCCC3)CC2)cc1
I-[CH;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1.[#7:6]1-[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]-1>>[#7:6]1-[C:7]-[C:8]-[N;H0;D3;+0:9](-[CH;D3;+0:1]2-[C:2]-[C:3]-[C:4]-[C:5]-2)-[C:10]-[C:11]-1
null
[]
null
null
null
null
A mixture of 1-(4-nitrophenyl)piperazine (12 g, 57.9 mmol) (Acros Organics), powdered potassium carbonate (5.4 g, 39 mmol), iodocyclopentane (7 mL, 60.8 mmol) (Aldrich) and a catalytic amount of 18-crown-6 in acetonitrile (90 mL) was heated at reflux overnight. The mixture was filtered, and the filter cake was washed w...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Secondary amine
Tertiary amine
C1CCCC1.C1C[NH]CCN1
C1C[NH]CC[NH]1.C1CCCC1
c1ccccc1.C1C[NH]CC[NH]1.C1CCCC1
HI
C(C)#N
null
null
IC1CCCC1.O=[N+]([O-])c1ccc(N2CCNCC2)cc1>C(C)#N>O=[N+]([O-])c1ccc(N2CCN(C3CCCC3)CC2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-712de18a6af24ee08e2c057d57d8ba1f
Nc1ccc(N2CCN(C3CCCC3)CC2)cc1.S=C(n1ccnc1)n1ccnc1>>S=C=Nc1ccc(N2CCN(C3CCCC3)CC2)cc1
C1(CCCC1)N1CCN(CC1)C1=CC=C(C=C1)N.C(=S)(N1C=NC=C1)N1C=NC=C1>>C1(CCCC1)N1CCN(CC1)C1=CC=C(C=C1)N=C=S
[NH2:3][c:4]1[cH:5][cH:6][c:7]([N:8]2[CH2:9][CH2:10][N:11]([CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16]3)[CH2:17][CH2:18]2)[cH:19][cH:20]1.c1cn([C:2](n2ccnc2)=[S:1])cn1>>[S:1]=[C:2]=[N:3][c:4]1[cH:5][cH:6][c:7]([N:8]2[CH2:9][CH2:10][N:11]([CH:12]3[CH2:13][CH2:14][CH2:15][CH2:16]3)[CH2:17][CH2:18]2)[cH:19][cH:20]1
Nc1ccc(N2CCN(C3CCCC3)CC2)cc1.S=C(n1ccnc1)n1ccnc1
S=C=Nc1ccc(N2CCN(C3CCCC3)CC2)cc1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCN(C3CCCC3)CC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
93.2
[{"value": 93.0, "product": "C1(CCCC1)N1CCN(CC1)C1=CC=C(C=C1)N=C=S", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.2, "product": "C1(CCCC1)N1CCN(CC1)C1=CC=C(C=C1)N=C=S", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-15
CELSIUS
20
MINUTE
A solution of 4-[4-(1-cyclopentyl)-1-piperazinyl]benzenamine (5.7 g, 22.4 mmol) (from Step B above) in N,N-dimethylformamide (75 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (4 g, 22.5 mmol) (Aldrich) in N,N-dimethylformamide (40 mL). After the addition was complete, the ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
c1ccccc1.C1C[NH]CC[NH]1.C1CCCC1
Other
CN(C=O)C
-15
0.333333
Nc1ccc(N2CCN(C3CCCC3)CC2)cc1.S=C(n1ccnc1)n1ccnc1>CN(C=O)C>S=C=Nc1ccc(N2CCN(C3CCCC3)CC2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4754a8151d09420396863f18deb623d8
CC(C)CI.O=[N+]([O-])c1ccc(N2CCNCC2)cc1>>CC(C)CN1CCN(c2ccc([N+](=O)[O-])cc2)CC1
[N+](=O)([O-])C1=CC=C(C=C1)N1CCNCC1.C([O-])([O-])=O.[K+].[K+].ICC(C)C.C1COCCOCCOCCOCCOCCO1>>C(C(C)C)N1CCN(CC1)C1=CC=C(C=C1)[N+](=O)[O-]
I[CH2:4][CH:2]([CH3:1])[CH3:3].[NH:5]1[CH2:6][CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([N+:13](=[O:14])[O-:15])[cH:16][cH:17]2)[CH2:18][CH2:19]1>>[CH3:1][CH:2]([CH3:3])[CH2:4][N:5]1[CH2:6][CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([N+:13](=[O:14])[O-:15])[cH:16][cH:17]2)[CH2:18][CH2:19]1
CC(C)CI.O=[N+]([O-])c1ccc(N2CCNCC2)cc1
CC(C)CN1CCN(c2ccc([N+](=O)[O-])cc2)CC1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
bad6b7d8e43c3debef0c262d60564e43415b41bcee72e526419c8c16be18fec1
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(N2CCNCC2)cc1
I-[CH2;D2;+0:1]-[C:2](-[C;D1;H3:3])-[C;D1;H3:4].[#7:5]1-[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]-1>>[C;D1;H3:3]-[C:2](-[C;D1;H3:4])-[CH2;D2;+0:1]-[N;H0;D3;+0:8]1-[C:7]-[C:6]-[#7:5]-[C:10]-[C:9]-1
null
[]
null
null
null
null
A mixture of 1-(4-nitrophenyl)piperazine (8 g, 38.6 mmol) (Acros Organics), powdered potassium carbonate (3.58 g, 25.98 mmol), 1-Iodo-2-methylpropane (4.66 ml, 40.5 mmol), and a catalytic amount of 18-crown-6 in acetonitrile (60 mL) was heated at reflux overnight. The mixture was filtered, and the filter cake was washe...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CNCC[NH]1
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1ccccc1
HI
C(C)#N
null
null
CC(C)CI.O=[N+]([O-])c1ccc(N2CCNCC2)cc1>C(C)#N>CC(C)CN1CCN(c2ccc([N+](=O)[O-])cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-62e20fc7b1c54fb7b05947ef301d624f
CC(C)CN1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>>CC(C)CN1CCN(c2ccc(N=C=S)cc2)CC1
C(C(C)C)N1CCN(CC1)C1=CC=C(C=C1)N.C(=S)(N1C=NC=C1)N1C=NC=C1>>N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC(C)C
[CH3:1][CH:2]([CH3:3])[CH2:4][N:5]1[CH2:6][CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([NH2:13])[cH:16][cH:17]2)[CH2:18][CH2:19]1.c1cn([C:14](n2ccnc2)=[S:15])cn1>>[CH3:1][CH:2]([CH3:3])[CH2:4][N:5]1[CH2:6][CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([N:13]=[C:14]=[S:15])[cH:16][cH:17]2)[CH2:18][CH2:19]1
CC(C)CN1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1
CC(C)CN1CCN(c2ccc(N=C=S)cc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCNCC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
87
[{"value": 87.0, "product": "N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.0, "product": "N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-15
CELSIUS
20
MINUTE
A solution of 4-[4-(isobutyl)-1-piperazinyl]benzenamine (7.8 g, 33.4 mmol) (from Step B above) in N,N-dimethylformamide (75 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (5.97 g, 33.5 mmol) (Aldrich) in N,N-dimethylformamide (25 mL). After the addition was complete, the mi...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
C1C[NH]CC[NH]1.c1ccccc1
Other
CN(C=O)C
-15
0.333333
CC(C)CN1CCN(c2ccc(N)cc2)CC1.S=C(n1ccnc1)n1ccnc1>CN(C=O)C>CC(C)CN1CCN(c2ccc(N=C=S)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-73aec980c739465dae1d7432720481ad
O=[N+]([O-])c1ccc(N2CCN(CCCO)CC2)cc1.[N-]=C=S>>OCCCN1CCN(c2ccc(N=C=S)cc2)CC1
[N+](=O)([O-])C1=CC=C(C=C1)N1CCN(CC1)CCCO.[N-]=C=S>>OCCCN1CCN(CC1)C1=CC=C(C=C1)N=C=S
O=[N+]([O-])[c:12]1[cH:11][cH:10][c:9]([N:8]2[CH2:7][CH2:6][N:5]([CH2:4][CH2:3][CH2:2][OH:1])[CH2:19][CH2:18]2)[cH:17][cH:16]1.[N-:13]=[C:14]=[S:15]>>[OH:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([N:13]=[C:14]=[S:15])[cH:16][cH:17]2)[CH2:18][CH2:19]1
O=[N+]([O-])c1ccc(N2CCN(CCCO)CC2)cc1.[N-]=C=S
OCCCN1CCN(c2ccc(N=C=S)cc2)CC1
null
null
null
Functional Group Interconversion
OtherReaction
c2b664bf7684468a37396b968ac0af317a7e2289f2edcfb8b7ab78ab404e94b4
305b6f3127a1d497f5798d688e7949ef02b1f99b0e5e183d105619e0875515fa
c1ccc(N2CCNCC2)cc1
O=[N+](-[O-])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[N-;H0;D1:6]=[C:7]=[S;D1;H0:8]>>[S;D1;H0:8]=[C:7]=[N;H0;D2;+0:6]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
null
null
This compound was prepared from 4-(4-nitrophenyl)-1-piperazinepropanol (which can be prepared according to the procedure of Loewe and Mieth Arzneim.-Forsch. 1966, 16, 1306–1310) using the hydrogenation and isothiocyanate-forming reactions used in Example 4. MS (ES) MH+=277. Conditions: See reaction.notes.procedure_deta...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Isothiocyanate
c1ccccc1
c1ccccc1
C1C[NH]CC[NH]1.c1ccccc1
Other
null
null
null
O=[N+]([O-])c1ccc(N2CCN(CCCO)CC2)cc1.[N-]=C=S>>OCCCN1CCN(c2ccc(N=C=S)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-604b53f6ab9a40748ebb4ec414303e96
Nc1ccc(N2CCN(CC3CC3)CC2)cc1.S=C(n1ccnc1)n1ccnc1>>S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
C1(CC1)CN1CCN(CC1)C1=CC=C(C=C1)N.C(=S)(N1C=NC=C1)N1C=NC=C1>>N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1
[NH2:3][c:4]1[cH:5][cH:6][c:7]([N:8]2[CH2:9][CH2:10][N:11]([CH2:12][CH:13]3[CH2:14][CH2:15]3)[CH2:16][CH2:17]2)[cH:18][cH:19]1.c1cn([C:2](n2ccnc2)=[S:1])cn1>>[S:1]=[C:2]=[N:3][c:4]1[cH:5][cH:6][c:7]([N:8]2[CH2:9][CH2:10][N:11]([CH2:12][CH:13]3[CH2:14][CH2:15]3)[CH2:16][CH2:17]2)[cH:18][cH:19]1
Nc1ccc(N2CCN(CC3CC3)CC2)cc1.S=C(n1ccnc1)n1ccnc1
S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
be7cda7c305cb7fe0f9c01bbc607472f3b10db5b9ac4c3f6176bd6d49196c1b0
b9d004d515d4691c0e9944172fdecaa5dd531c6cfbffee450da8866f92f0f7d4
c1ccc(N2CCN(CC3CC3)CC2)cc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[S;D1;H0:5]=[C;H0;D3;+0:6](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[S;D1;H0:5]=[C;H0;D2;+0:6]=[N;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
-15
CELSIUS
20
MINUTE
A solution of 4-[4-(cyclopropylmethyl)-1-piperazinyl]benzenamine (3.7 g, 16 mmol) (from Step B above) in N,N-dimethylformamide (50 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (2.87 g, 16.1 mmol) (Aldrich) in N,N-dimethylformamide (25 mL). After the addition was complete,...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Thiocarbonyl
Isothiocyanate
c1c[nH]cn1.c1c[nH]cn1
null
c1ccccc1.C1C[NH]CC[NH]1.C1CC1
Other
CN(C=O)C
-15
0.333333
Nc1ccc(N2CCN(CC3CC3)CC2)cc1.S=C(n1ccnc1)n1ccnc1>CN(C=O)C>S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-df8740b33601414ebe721ffc9cf8e541
BrBr.CCc1cccc(C(C)=O)c1>>CCc1cccc(C(=O)CBr)c1
CCC1=CC=CC(=C1)C(=O)C.BrBr>>BrCC(=O)C1=CC(=CC=C1)CC
Br[Br:11].[CH3:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8](=[O:9])[CH3:10])[cH:12]1>>[CH3:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8](=[O:9])[CH2:10][Br:11])[cH:12]1
BrBr.CCc1cccc(C(C)=O)c1
CCc1cccc(C(=O)CBr)c1
null
null
O1CCOCC1
Functional Group Interconversion
Bromination
97ca6720945af5a02c450d33ec56e946521050f9771c27f9cfcb85f3477593f6
cb3e14519230141aa015a4cf9c960def3e60f01997e61621f62506924bfa15de
c1ccccc1
Br-[Br;H0;D1;+0:1].[CH3;D1;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3](=[O;D1;H0:4])-[c:5]
68.1
[{"value": 68.0, "product": "BrCC(=O)C1=CC(=CC=C1)CC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 68.1, "product": "BrCC(=O)C1=CC(=CC=C1)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a stirred solution of 3-ethylacetophenone (Maybridge Chemical Company Ltd.; 1.103 g, 7.44 mmol) in dry 1,4-dioxane (15 mL) was added bromine (383 μL, 7.44 mmol). The solution was stirred at room temperature for 30 min. and then the solvent was removed on a rotary evaporator. The residue was chromatographed on a Foxy...
10.6084/m9.figshare.5104873.v1
null
Ketone
Primary halide
null
null
c1ccccc1
HBr
O1CCOCC1
null
0.5
BrBr.CCc1cccc(C(C)=O)c1>O1CCOCC1>CCc1cccc(C(=O)CBr)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0ed24783b19a418792f2d568d95728e8
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc(Cl)c([N+](=O)[O-])c1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1
BrCC(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-].N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C.N#CN.CC(C)([O-])C.[K+]>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:28])[cH:29][cH:30]2)[CH2:31][CH2:32]1.[NH2:12][C:13]#[N:14].Br[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][c:21]([Cl:22])[c:23]([N+:24](=[O:25])[O-:26])[cH:27]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH:10][c:11]3[n:12][c:13](...
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc(Cl)c([N+](=O)[O-])c1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1
null
null
O.C(C)#N
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
45
[{"value": 45.0, "product": "NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 44.3, "product": "NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a mixture of 1-(4-isothiocyanatophenyl)-4-methylpiperazine (of Example 1; 1.0 g, 4.3 mmol) and cyanamide (0.2 g, 4.8 mmol) in acetonitrile (43 mL), a solution of potassium tert-butoxide (43 mL, 0.1 M in tert-BuOH) was added. After 30 minutes at room temperature, 2-bromo-1-(4-chloro-3-nitro-phenyl)ethanone (1.2 g, 4....
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1
HBr
O.C(C)#N
null
0.5
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc(Cl)c([N+](=O)[O-])c1>O.C(C)#N>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4444a9b30ad444b689cb68b79a2ae3f2
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc2c(c1)OCCO2>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc5c(c4)OCCO5)s3)cc2)CC1
BrCC(=O)C1=CC2=C(OCCO2)C=C1.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C.N#CN.CC(C)([O-])C.[K+]>>NC=1N=C(SC1C(=O)C1=CC2=C(OCCO2)C=C1)NC1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:28])[cH:29][cH:30]2)[CH2:31][CH2:32]1.[NH2:12][C:13]#[N:14].Br[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][c:21]2[c:22]([cH:23]1)[O:24][CH2:25][CH2:26][O:27]2>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH:10][c:11]3[n:12][c:13]([N...
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc2c(c1)OCCO2
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc5c(c4)OCCO5)s3)cc2)CC1
null
null
C(C)(C)(C)O.C(C)#N
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccc2c(c1)OCCO2)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
66
[{"value": 66.0, "product": "NC=1N=C(SC1C(=O)C1=CC2=C(OCCO2)C=C1)NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.0, "product": "NC=1N=C(SC1C(=O)C1=CC2=C(OCCO2)C=C1)NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
tert-Butanol (4 mL) and then 1-(4-isothiocyanatophenyl)-4-methyl piperazine (of Example 1; 219 mg, 1 mmol) were added to a solution of cyanamide (44 mg, 1.05 mmol) (Aldrich) in acetonitrile (5 mL). Potassium t-butoxide (1 M in tert-butanol; 1 mL, 1 mmol) was added and the solution was stirred for 30 min. 2-Bromo-1-(2,3...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccc2c(c1)OCCO2
HBr
C(C)(C)(C)O.C(C)#N
null
0.5
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc2c(c1)OCCO2>C(C)(C)(C)O.C(C)#N>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc5c(c4)OCCO5)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e2adeb5088e848eab7be6471672b965b
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc2c(c1)OCO2>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc5c(c4)OCO5)s3)cc2)CC1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C.O1COC2=C1C=CC(=C2)C(CBr)=O>>NC=1N=C(SC1C(=O)C1=CC2=C(OCO2)C=C1)NC1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:27])[cH:28][cH:29]2)[CH2:30][CH2:31]1.[NH2:12][C:13]#[N:14].Br[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][c:21]2[c:22]([cH:23]1)[O:24][CH2:25][O:26]2>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH:10][c:11]3[n:12][c:13]([NH2:14])[...
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc2c(c1)OCO2
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc5c(c4)OCO5)s3)cc2)CC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccc2c(c1)OCO2)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
75
[{"value": 75.0, "product": "NC=1N=C(SC1C(=O)C1=CC2=C(OCO2)C=C1)NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
This compound was prepared in 75% yield from cyanamide (Aldrich), 1-(4-isothiocyanatophenyl)-4-methylpiperazine (of Example 1), and 1-(1,3-benzodioxol-5-yl)-2-bromoethanone (of Example 11) following the procedure used to in Example 24. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccc2c(c1)OCO2
HBr
null
null
null
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc2c(c1)OCO2>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc5c(c4)OCO5)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b17a0c7b6d284d0a959d2f696bb214cf
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc(N2CCCC2)cc1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC5)cc4)s3)cc2)CC1
BrCC(=O)C1=CC=C(C=C1)N1CCCC1.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C.N#CN.CC(C)([O-])C.[K+]>>NC=1N=C(SC1C(=O)C1=CC=C(C=C1)N1CCCC1)NC1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:29])[cH:30][cH:31]2)[CH2:32][CH2:33]1.[NH2:12][C:13]#[N:14].Br[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][c:21]([N:22]2[CH2:23][CH2:24][CH2:25][CH2:26]2)[cH:27][cH:28]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH:10][c:11]3[n:1...
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc(N2CCCC2)cc1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC5)cc4)s3)cc2)CC1
null
null
C(C)(C)(C)O.C(C)#N
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccc(N2CCCC2)cc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
4
[{"value": 4.0, "product": "NC=1N=C(SC1C(=O)C1=CC=C(C=C1)N1CCCC1)NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
tert-Butanol (4 mL) and then 1-(4-isothiocyanatophenyl)-4-methyl piperazine (of Example 1; 219 mg, 1 mmol) were added to a solution of cyanamide (44 mg, 1.05 mmol) in acetonitrile (5 mL). Potassium t-butoxide (1 M in tert-butanol; 1 mL, 1 mmol) was added and the solution was stirred for 30 min. 2-Bromo-1-[4-(1-pyrrolid...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1.C1CC[NH]C1
HBr
C(C)(C)(C)O.C(C)#N
null
0.5
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1ccc(N2CCCC2)cc1>C(C)(C)(C)O.C(C)#N>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC5)cc4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e78d3b5aa11a457f95286fc7827ae285
CC(C)(C)OC(=O)N1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(F)c4)s3)cc2)CC1>>Nc1nc(Nc2ccc(N3CCNCC3)cc2)sc1C(=O)c1cccc(F)c1
NC=1N=C(SC1C(C1=CC(=CC=C1)F)=O)NC1=CC=C(C=C1)N1CCN(CC1)C(=O)OC(C)(C)C.C(=O)(C(F)(F)F)O.C(Cl)Cl>>NC=1N=C(SC1C(=O)C1=CC(=CC=C1)F)NC1=CC=C(C=C1)N1CCNCC1
CC(C)(C)OC(=O)[N:13]1[CH2:12][CH2:11][N:10]([c:9]2[cH:8][cH:7][c:6]([NH:5][c:4]3[n:3][c:2]([NH2:1])[c:19]([C:20](=[O:21])[c:22]4[cH:23][cH:24][cH:25][c:26]([F:27])[cH:28]4)[s:18]3)[cH:17][cH:16]2)[CH2:15][CH2:14]1>>[NH2:1][c:2]1[n:3][c:4]([NH:5][c:6]2[cH:7][cH:8][c:9]([N:10]3[CH2:11][CH2:12][NH:13][CH2:14][CH2:15]3)[cH...
CC(C)(C)OC(=O)N1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(F)c4)s3)cc2)CC1
Nc1nc(Nc2ccc(N3CCNCC3)cc2)sc1C(=O)c1cccc(F)c1
null
null
null
Reduction
Boc amine deprotection
2c25e19aee181a3c5131cfdfda27035fd54d4379a11d745dfb75d386bacfd500
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1>>[#7:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:6]-[C:5]-1
100.6
[{"value": 100.0, "product": "NC=1N=C(SC1C(=O)C1=CC(=CC=C1)F)NC1=CC=C(C=C1)N1CCNCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 100.6, "product": "NC=1N=C(SC1C(=O)C1=CC(=CC=C1)F)NC1=CC=C(C=C1)N1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A mixture of 4-[4-[[4-amino-5-(3-fluorobenzoyl)-2-thiazolyl]amino]phenyl]1-piperazinec acid, 1,1-dimethylethyl ester (75 mg, 0.15 mmol) (from Step A above) and a solution of TFA/CH2Cl2 (1:1; 1.5 mL) was gently shaken for 1.5 h. The solution was evaporated in vacuo. To the residue was added resin-bound N,N-diisopropylet...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1C[NH]CC[NH]1
C1C[NH]CCN1
c1cscn1.c1ccccc1.C1C[NH]CCN1.c1ccccc1
HO-
null
null
8
CC(C)(C)OC(=O)N1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(F)c4)s3)cc2)CC1>>Nc1nc(Nc2ccc(N3CCNCC3)cc2)sc1C(=O)c1cccc(F)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-514f448472b6432cb9ba9c7ab9748ad1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.NCCO>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(NCCO)c([N+](=O)[O-])c4)s3)cc2)CC1
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.C(O)CN.C(C)(C)N(C(C)C)CC>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)NCCO)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
Cl[c:21]1[cH:20][cH:19][c:18]([C:16]([c:15]2[c:13]([NH2:14])[n:12][c:11]([NH:10][c:9]3[cH:8][cH:7][c:6]([N:5]4[CH2:4][CH2:3][N:2]([CH3:1])[CH2:35][CH2:34]4)[cH:33][cH:32]3)[s:31]2)=[O:17])[cH:30][c:26]1[N+:27](=[O:28])[O-:29].[NH2:22][CH2:23][CH2:24][OH:25]>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH:...
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.NCCO
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(NCCO)c([N+](=O)[O-])c4)s3)cc2)CC1
null
null
C(CCC)O
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:9]-[C:8]-[C:7]):[c:2]:[c:3]
28
[{"value": 28.0, "product": "NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)NCCO)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 27.7, "product": "NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)NCCO)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
A mixture of [4-amino-2-[[4-(4-methyl-1-piperazinyl)phenyl]amino]-5-thiazolyl](4-chloro-3-nitrophenyl)methanone (of Example 15; 0.25 g, 0.53 mmol), ethanolamine (0.13 mL, 2.12 mmol), N,N-diisopropylethylamine (Aldrich) (0.37 mL, 2.12 mmol) in n-butanol (10 mL) was heated at 100° C. overnight. The solvent was evaporated...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1
HCl
C(CCC)O
100
null
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.NCCO>C(CCC)O>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(NCCO)c([N+](=O)[O-])c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b309a51fb6514b5eb56f5989cdb84e32
C1CCNC1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC5)c([N+](=O)[O-])c4)s3)cc2)CC1
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.N1CCCC1>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)N1CCCC1)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
[NH:22]1[CH2:23][CH2:24][CH2:25][CH2:26]1.Cl[c:21]1[cH:20][cH:19][c:18]([C:16]([c:15]2[c:13]([NH2:14])[n:12][c:11]([NH:10][c:9]3[cH:8][cH:7][c:6]([N:5]4[CH2:4][CH2:3][N:2]([CH3:1])[CH2:36][CH2:35]4)[cH:34][cH:33]3)[s:32]2)=[O:17])[cH:31][c:27]1[N+:28](=[O:29])[O-:30]>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8]...
C1CCNC1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC5)c([N+](=O)[O-])c4)s3)cc2)CC1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
389dbc6c760ba22d5b089335787069e4da1dc4ed4889d745a0e1de1824c34c09
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
O=C(c1ccc(N2CCCC2)cc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]1-[C:8]-[C:9]-[C:10]-[NH;D2;+0:11]-1>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[N;H0;D3;+0:11]1-[C:7]-[C:8]-[C:9]-[C:10]-1):[c:2]:[c:3]
null
[]
null
null
null
null
This compound was prepared from the compound of Example 15 and pyrrolidine by the procedure used in Example 57. Mass spectrum (ES) MH+=508. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CCNC1.c1ccccc1
c1ccccc1.C1CC[NH]C1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1.C1CC[NH]C1
HCl
null
null
null
C1CCNC1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC5)c([N+](=O)[O-])c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e55884b8a1844eb0851cd06728910c98
C1COCCN1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCOCC5)c([N+](=O)[O-])c4)s3)cc2)CC1
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.N1CCOCC1>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)N1CCOCC1)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
[NH:22]1[CH2:23][CH2:24][O:25][CH2:26][CH2:27]1.Cl[c:21]1[cH:20][cH:19][c:18]([C:16]([c:15]2[c:13]([NH2:14])[n:12][c:11]([NH:10][c:9]3[cH:8][cH:7][c:6]([N:5]4[CH2:4][CH2:3][N:2]([CH3:1])[CH2:37][CH2:36]4)[cH:35][cH:34]3)[s:33]2)=[O:17])[cH:32][c:28]1[N+:29](=[O:30])[O-:31]>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7]...
C1COCCN1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCOCC5)c([N+](=O)[O-])c4)s3)cc2)CC1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
a47b7d43ef99c1989f39629bd45f903079b03ac5a9d702fdbffdae93a63a79cd
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
O=C(c1ccc(N2CCOCC2)cc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[#8:7]1-[C:8]-[C:9]-[NH;D2;+0:10]-[C:11]-[C:12]-1>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[N;H0;D3;+0:10]1-[C:9]-[C:8]-[#8:7]-[C:12]-[C:11]-1):[c:2]:[c:3]
null
[]
null
null
null
null
This compound was prepared from the compound of Example 15 and morpholine by the procedure used in Example 57. Mass spectrum (ES) MH+=524. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1COCCN1.c1ccccc1
c1ccccc1.C1COCC[NH]1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1.C1COCC[NH]1
HCl
null
null
null
C1COCCN1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCOCC5)c([N+](=O)[O-])c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1525708d3c8442e29f890fe73ad50d45
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.COCCN>>COCCNc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.COCCN>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)NCCOC)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
Cl[c:6]1[cH:7][cH:8][c:9]([C:10](=[O:11])[c:12]2[s:13][c:14]([NH:15][c:16]3[cH:17][cH:18][c:19]([N:20]4[CH2:21][CH2:22][N:23]([CH3:24])[CH2:25][CH2:26]4)[cH:27][cH:28]3)[n:29][c:30]2[NH2:31])[cH:32][c:33]1[N+:34](=[O:35])[O-:36].[CH3:1][O:2][CH2:3][CH2:4][NH2:5]>>[CH3:1][O:2][CH2:3][CH2:4][NH:5][c:6]1[cH:7][cH:8][c:9](...
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.COCCN
COCCNc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:9]-[C:8]-[C:7]):[c:2]:[c:3]
null
[]
null
null
null
null
This compound was prepared from the compound of Example 15 and 2-methoxyethanamine (Aldrich) by the procedure used in Example 57. Mass spectrum (ES) MH+=512. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1cscn1.c1ccccc1.C1C[NH]CC[NH]1
HCl
null
null
null
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.COCCN>>COCCNc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d7b06ea0f2724bfb9e297e97cd7e3e58
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.OCC1CCCNC1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC(CO)C5)c([N+](=O)[O-])c4)s3)cc2)CC1
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.N1CC(CCC1)CO>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)N1CC(CCC1)CO)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
Cl[c:21]1[cH:20][cH:19][c:18]([C:16]([c:15]2[c:13]([NH2:14])[n:12][c:11]([NH:10][c:9]3[cH:8][cH:7][c:6]([N:5]4[CH2:4][CH2:3][N:2]([CH3:1])[CH2:39][CH2:38]4)[cH:37][cH:36]3)[s:35]2)=[O:17])[cH:34][c:30]1[N+:31](=[O:32])[O-:33].[NH:22]1[CH2:23][CH2:24][CH2:25][CH:26]([CH2:27][OH:28])[CH2:29]1>>[CH3:1][N:2]1[CH2:3][CH2:4]...
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.OCC1CCCNC1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC(CO)C5)c([N+](=O)[O-])c4)s3)cc2)CC1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
ad5ec9c4592e4dee5877fc4f1309a503a378773e18ebc21adf780b709f6e28c5
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
O=C(c1ccc(N2CCCCC2)cc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[N;H0;D3;+0:9](-[C:8]-[C:7])-[C:10]-[C:11]):[c:2]:[c:3]
null
[]
null
null
null
null
This compound was prepared from the compound of Example 15 and racemic 3-piperidinemethanol (Aldrich) by the procedure used in Example 57. Mass spectrum (ES) MH+=552. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
c1ccccc1.C1CCNCC1
c1ccccc1.C1CC[NH]CC1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1.C1CC[NH]CC1
HCl
null
null
null
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.OCC1CCCNC1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCCC(CO)C5)c([N+](=O)[O-])c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f71ea8aaf3d74f99a567d56fac4f7b4d
CC1CCCN1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1>>CC1CCCN1c1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.CC1NCCC1>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)N1C(CCC1)C)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][NH:6]1.Cl[c:7]1[cH:8][cH:9][c:10]([C:11](=[O:12])[c:13]2[s:14][c:15]([NH:16][c:17]3[cH:18][cH:19][c:20]([N:21]4[CH2:22][CH2:23][N:24]([CH3:25])[CH2:26][CH2:27]4)[cH:28][cH:29]3)[n:30][c:31]2[NH2:32])[cH:33][c:34]1[N+:35](=[O:36])[O-:37]>>[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]1[c:7]...
CC1CCCN1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1
CC1CCCN1c1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
389dbc6c760ba22d5b089335787069e4da1dc4ed4889d745a0e1de1824c34c09
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
O=C(c1ccc(N2CCCC2)cc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C;D1;H3:7]-[C:8]1-[C:9]-[C:10]-[C:11]-[NH;D2;+0:12]-1>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[N;H0;D3;+0:12]1-[C:11]-[C:10]-[C:9]-[C:8]-1-[C;D1;H3:7]):[c:2]:[c:3]
null
[]
null
null
null
null
This compound was prepared from the compound of Example 15 and racemic 2-methylpyrrolidine (Alfa Aesar) by the procedure used in Example 57. Mass spectrum (ES) MH+=522. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CCNC1.c1ccccc1
C1CC[NH]C1.c1ccccc1
C1CC[NH]C1.c1ccccc1.c1cscn1.c1ccccc1.C1C[NH]CC[NH]1
HCl
null
null
null
CC1CCCN1.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1>>CC1CCCN1c1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bf0a53130d38412282e165d28ddfe4be
CC(C)C[C@@H](N)CO.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1>>CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.N[C@@H](CO)CC(C)C>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)N[C@H](CC(C)C)CO)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][CH:2]([CH3:3])[CH2:4][C@H:5]([CH2:6][OH:7])[NH2:8].Cl[c:9]1[cH:10][cH:11][c:12]([C:13](=[O:14])[c:15]2[s:16][c:17]([NH:18][c:19]3[cH:20][cH:21][c:22]([N:23]4[CH2:24][CH2:25][N:26]([CH3:27])[CH2:28][CH2:29]4)[cH:30][cH:31]3)[n:32][c:33]2[NH2:34])[cH:35][c:36]1[N+:37](=[O:38])[O-:39]>>[CH3:1][CH:2]([CH3:3])[CH2:4...
CC(C)C[C@@H](N)CO.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1
CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8](-[C:9])-[NH2;D1;+0:10]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:10]-[C:8](-[C:7])-[C:9]):[c:2]:[c:3]
null
[]
null
null
null
null
This compound was prepared from the compound of Example 15 and (R)-2-amino-4-methyl-1-pentanol (Aldrich) by the procedure used in Example 57. Mass spectrum (ES) MH+=554. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1cscn1.c1ccccc1.C1C[NH]CC[NH]1
HCl
null
null
null
CC(C)C[C@@H](N)CO.CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1>>CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a190f012b2de44119320ad4ef6789f10
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.OC1CCNCC1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCC(O)CC5)c([N+](=O)[O-])c4)s3)cc2)CC1
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)Cl)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.N1CCC(CC1)O>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)N1CCC(CC1)O)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C
Cl[c:21]1[cH:20][cH:19][c:18]([C:16]([c:15]2[c:13]([NH2:14])[n:12][c:11]([NH:10][c:9]3[cH:8][cH:7][c:6]([N:5]4[CH2:4][CH2:3][N:2]([CH3:1])[CH2:38][CH2:37]4)[cH:36][cH:35]3)[s:34]2)=[O:17])[cH:33][c:29]1[N+:30](=[O:31])[O-:32].[NH:22]1[CH2:23][CH2:24][CH:25]([OH:26])[CH2:27][CH2:28]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c...
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.OC1CCNCC1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCC(O)CC5)c([N+](=O)[O-])c4)s3)cc2)CC1
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
ad5ec9c4592e4dee5877fc4f1309a503a378773e18ebc21adf780b709f6e28c5
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
O=C(c1ccc(N2CCCCC2)cc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[N;H0;D3;+0:9](-[C:8]-[C:7])-[C:10]-[C:11]):[c:2]:[c:3]
null
[]
null
null
null
null
This compound was prepared from the compound of Example 15 and 4-piperidinol (Aldrich) by the procedure used in Example 57. Mass spectrum (ES) MH+=538. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
c1ccccc1.C1CCNCC1
c1ccccc1.C1CC[NH]CC1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1.C1CC[NH]CC1
HCl
null
null
null
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(Cl)c([N+](=O)[O-])c4)s3)cc2)CC1.OC1CCNCC1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4ccc(N5CCC(O)CC5)c([N+](=O)[O-])c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e22344accb1d4910a848b743bfa211d1
CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]>>CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1N
NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)N[C@H](CC(C)C)CO)[N+](=O)[O-])NC1=CC=C(C=C1)N1CCN(CC1)C.NN.CC(C)O>>NC=1C=C(C=CC1N[C@H](CC(C)C)CO)C(=O)C1=C(N=C(S1)NC1=CC=C(C=C1)N1CCN(CC1)C)N
O=[N+:37]([O-])[c:36]1[c:9]([NH:8][C@H:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[CH2:6][OH:7])[cH:10][cH:11][c:12]([C:13](=[O:14])[c:15]2[s:16][c:17]([NH:18][c:19]3[cH:20][cH:21][c:22]([N:23]4[CH2:24][CH2:25][N:26]([CH3:27])[CH2:28][CH2:29]4)[cH:30][cH:31]3)[n:32][c:33]2[NH2:34])[cH:35]1>>[CH3:1][CH:2]([CH3:3])[CH2:4][C@H:5]([...
CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]
CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1N
null
[Pd]
ClCCl.CO
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
57.3
[{"value": 53.0, "product": "NC=1C=C(C=CC1N[C@H](CC(C)C)CO)C(=O)C1=C(N=C(S1)NC1=CC=C(C=C1)N1CCN(CC1)C)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 57.3, "product": "NC=1C=C(C=CC1N[C@H](CC(C)C)CO)C(=O)C1=C(N=C(S1)NC1=CC=C(C=C1)N1CCN(CC1)C)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of (R)-[4-amino-2-[[4-(4-methyl-1-piperazinyl)phenyl]amino]-5-thiazolyl][3-nitro-4-[[1-(hydroxymethyl)-3-methylbutyl]amino]phenyl]methanone (of Example 63; 30 mg, 0.05 mmol), NH2NH2 (0.5 mL), 10% Pd/C (5 mg), and 2-propanol (2 mL) was heated at reflux for 1 h. The mixture was filtered through a Celite™ pad a...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1cscn1.c1ccccc1.C1C[NH]CC[NH]1
Other
[Pd].ClCCl.CO
null
null
CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1[N+](=O)[O-]>[Pd].ClCCl.CO>CC(C)C[C@H](CO)Nc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)cc1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-84efb16b6cff4ea9853c2e13e6553a50
O=P(O)(O)O>>O=P(O)(O)O
NC=1N=C(SC1C(=O)C1=CC(=CC=C1)OC)NC1=CC=C(C=C1)N1CCN(CC1)C(C)C.P(O)(O)(O)=O>>P(O)(O)(O)=O.NC=1N=C(SC1C(=O)C1=CC(=CC=C1)OC)NC1=CC=C(C=C1)N1CCN(CC1)C(C)C
[O:33]=[P:34]([OH:35])([OH:36])[OH:37]>>[O:33]=[P:34]([OH:35])([OH:36])[OH:37]
O=P(O)(O)O
O=P(O)(O)O
null
null
C(C)O
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
null
null
null
null
A solution of {4-amino-2-[4-(4-isopropyl-piperazin-1-yl)-phenylamino]-thiazol-5-yl}-(3-methoxy-phenyl)-methanone (of Example 43; 113 mg, 0.25 mmol) was dissolved in hot ethanol (10 ml) and to this was added 25 mg of phosphoric acid in ethanol (1 ml). This was cooled and crystals were collected and dried to furnish {4-A...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
C(C)O
null
null
O=P(O)(O)O>C(C)O>O=P(O)(O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-eeb6facdc8e0446389e7e7456b4ead4b
CN1CCN(c2ccc(N=C=S)cc2)CC1.CSc1cccc(C(=O)CBr)c1.N#CN>>CSc1cccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)c1
BrCC(=O)C1=CC(=CC=C1)SC.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C.N#CN.CC(C)([O-])C.[K+]>>NC=1N=C(SC1C(=O)C1=CC(=CC=C1)SC)NC1=CC=C(C=C1)N1CCN(CC1)C
[S:11]=[C:12]=[N:13][c:14]1[cH:15][cH:16][c:17]([N:18]2[CH2:19][CH2:20][N:21]([CH3:22])[CH2:23][CH2:24]2)[cH:25][cH:26]1.Br[CH2:10][C:8]([c:7]1[cH:6][cH:5][cH:4][c:3]([S:2][CH3:1])[cH:30]1)=[O:9].[NH2:27][C:28]#[N:29]>>[CH3:1][S:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8](=[O:9])[c:10]2[s:11][c:12]([NH:13][c:14]3[cH:15][cH:1...
CN1CCN(c2ccc(N=C=S)cc2)CC1.CSc1cccc(C(=O)CBr)c1.N#CN
CSc1cccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)c1
null
null
C(C)(C)(C)O.C(C)(=O)OCC.C(C)#N
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
50
[{"value": 50.0, "product": "NC=1N=C(SC1C(=O)C1=CC(=CC=C1)SC)NC1=CC=C(C=C1)N1CCN(CC1)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a mixture of 1-(4-isothiocyanatophenyl)-4-methylpiperazine (of Example 1; 0.466 g, 2.0 mmol) and cyanamide (0.088 g, 2.1 mmol) in acetonitrile (3 mL) and t-butanol (5 ml), a solution of potassium tert-butoxide (2.0 mL, 1.0 M in tert-BuOH) was added. After 30 minutes at room temperature, 2-bromo-1-(3-methylsulfanyl-p...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
c1ccccc1.c1cscn1.c1ccccc1.C1C[NH]CC[NH]1
HBr
C(C)(C)(C)O.C(C)(=O)OCC.C(C)#N
null
0.5
CN1CCN(c2ccc(N=C=S)cc2)CC1.CSc1cccc(C(=O)CBr)c1.N#CN>C(C)(C)(C)O.C(C)(=O)OCC.C(C)#N>CSc1cccc(C(=O)c2sc(Nc3ccc(N4CCN(C)CC4)cc3)nc2N)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3c6803e0976a49bba12682bb51f30c25
CC(C)N1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.N#Cc1cccc(C(=O)CBr)c1>>CC(C)N1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(C#N)c4)s3)cc2)CC1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C(C)C.C(#N)C=1C=C(C(CBr)=O)C=CC1>>NC=1N=C(SC1C(=O)C=1C=C(C#N)C=CC1)NC1=CC=C(C=C1)N1CCN(CC1)C(C)C
[CH3:1][CH:2]([CH3:3])[N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([N:12]=[C:13]=[S:28])[cH:29][cH:30]2)[CH2:31][CH2:32]1.[NH2:14][C:15]#[N:16].Br[CH2:17][C:18](=[O:19])[c:20]1[cH:21][cH:22][cH:23][c:24]([C:25]#[N:26])[cH:27]1>>[CH3:1][CH:2]([CH3:3])[N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][c:11]([NH:12][c:1...
CC(C)N1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.N#Cc1cccc(C(=O)CBr)c1
CC(C)N1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(C#N)c4)s3)cc2)CC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-isopropypiperazine (of Example 3) and 3-cyanophenacyl bromide (Maybridge Chemical Co. Ltd.) following the procedure used in Example 24. Mass spectrum (ES) MH+=447. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1
HBr
null
null
null
CC(C)N1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.N#Cc1cccc(C(=O)CBr)c1>>CC(C)N1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(C#N)c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-613fa06c3fcd4a528f837a7497987e54
N#CN.O=C(CBr)c1cccc(OC(F)F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1cccc(OC(F)F)c1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1.BrCC(=O)C1=CC(=CC=C1)OC(F)F>>NC=1N=C(SC1C(=O)C1=CC(=CC=C1)OC(F)F)NC1=CC=C(C=C1)N1CCN(CC1)CC1CC1
[N:1]#[C:2][NH2:3].Br[CH2:23][C:24](=[O:25])[c:26]1[cH:27][cH:28][cH:29][c:30]([O:31][CH:32]([F:33])[F:34])[cH:35]1.[C:4](=[N:5][c:6]1[cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][N:13]([CH2:14][CH:15]3[CH2:16][CH2:17]3)[CH2:18][CH2:19]2)[cH:20][cH:21]1)=[S:22]>>[NH2:1][c:2]1[n:3][c:4]([NH:5][c:6]2[cH:7][cH:8][c:9]([N:10]3...
N#CN.O=C(CBr)c1cccc(OC(F)F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1cccc(OC(F)F)c1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-cyclopropylmethylpiperazine (of Example 14G) and 2-bromo-1-(3-difluoro-methoxyphenyl)ethanone (of Example 14L) following the procedure used in Example 24. Mass spectrum (ES) MH+=500. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
c1cscn1.c1ccccc1.C1C[NH]CC[NH]1.C1CC1.c1ccccc1
HBr
null
null
null
N#CN.O=C(CBr)c1cccc(OC(F)F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1cccc(OC(F)F)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-85ee76f1be514947a55c08761ca008f0
COc1cccc(C(=O)CBr)c1.N#CN.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>COc1cccc(C(=O)c2sc(Nc3ccc(N4CCN(CC5CC5)CC4)cc3)nc2N)c1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1.BrCC(=O)C1=CC(=CC=C1)OC>>NC=1N=C(SC1C(=O)C1=CC(=CC=C1)OC)NC1=CC=C(C=C1)N1CCN(CC1)CC1CC1
Br[CH2:10][C:8]([c:7]1[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[cH:33]1)=[O:9].[NH2:30][C:31]#[N:32].[S:11]=[C:12]=[N:13][c:14]1[cH:15][cH:16][c:17]([N:18]2[CH2:19][CH2:20][N:21]([CH2:22][CH:23]3[CH2:24][CH2:25]3)[CH2:26][CH2:27]2)[cH:28][cH:29]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8](=[O:9])[c:10]2[s:11][c:12]([...
COc1cccc(C(=O)CBr)c1.N#CN.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
COc1cccc(C(=O)c2sc(Nc3ccc(N4CCN(CC5CC5)CC4)cc3)nc2N)c1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-cyclopropylmethylpiperazine (of Example 14G) and 2-bromo-1-(3-methoxyphenyl)ethanone (Aldrich) following the procedure used in Example 24 Mass spectrum (ES) MH+=464. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
c1ccccc1.c1cscn1.c1ccccc1.C1C[NH]CC[NH]1.C1CC1
HBr
null
null
null
COc1cccc(C(=O)CBr)c1.N#CN.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>COc1cccc(C(=O)c2sc(Nc3ccc(N4CCN(CC5CC5)CC4)cc3)nc2N)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8d916d1a8d734bca8f579d63c504873f
N#CN.O=C(CBr)c1ccc2c(c1)OCO2.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc2c(c1)OCO2
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1.O1COC2=C1C=CC(=C2)C(CBr)=O>>NC=1N=C(SC1C(=O)C1=CC2=C(OCO2)C=C1)NC1=CC=C(C=C1)N1CCN(CC1)CC1CC1
[N:1]#[C:2][NH2:3].Br[CH2:23][C:24](=[O:25])[c:26]1[cH:27][cH:28][c:29]2[c:30]([cH:31]1)[O:32][CH2:33][O:34]2.[C:4](=[N:5][c:6]1[cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][N:13]([CH2:14][CH:15]3[CH2:16][CH2:17]3)[CH2:18][CH2:19]2)[cH:20][cH:21]1)=[S:22]>>[NH2:1][c:2]1[n:3][c:4]([NH:5][c:6]2[cH:7][cH:8][c:9]([N:10]3[CH2:1...
N#CN.O=C(CBr)c1ccc2c(c1)OCO2.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc2c(c1)OCO2
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccc2c(c1)OCO2)c1cnc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-cyclopropylmethylpiperazine (of Example 14G) and 2-bromo-[(benzo[1,3]dioxol-5-yl)ethanone (of Example 11) following the procedure used in Example 24 Mass spectrum (ES) MH+=478. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
c1cscn1.c1ccccc1.C1C[NH]CC[NH]1.C1CC1.c1ccc2c(c1)OCO2
HBr
null
null
null
N#CN.O=C(CBr)c1ccc2c(c1)OCO2.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc2c(c1)OCO2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d81c27ecaf974a728c8d06da8118a081
N#CN.O=C(CBr)c1ccc2c(c1)OCCO2.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc2c(c1)OCCO2
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1.BrCC(=O)C1=CC2=C(OCCO2)C=C1>>NC=1N=C(SC1C(=O)C1=CC2=C(OCCO2)C=C1)NC1=CC=C(C=C1)N1CCN(CC1)CC1CC1
[N:1]#[C:2][NH2:3].Br[CH2:23][C:24](=[O:25])[c:26]1[cH:27][cH:28][c:29]2[c:30]([cH:31]1)[O:32][CH2:33][CH2:34][O:35]2.[C:4](=[N:5][c:6]1[cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][N:13]([CH2:14][CH:15]3[CH2:16][CH2:17]3)[CH2:18][CH2:19]2)[cH:20][cH:21]1)=[S:22]>>[NH2:1][c:2]1[n:3][c:4]([NH:5][c:6]2[cH:7][cH:8][c:9]([N:10...
N#CN.O=C(CBr)c1ccc2c(c1)OCCO2.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc2c(c1)OCCO2
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccc2c(c1)OCCO2)c1cnc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-cyclopropylmethylpiperazine (of Example 14G) and 2-bromo-1-(2,3-dihydro-benzo[1,4]dioxin-6-yl)ethanone (Maybridge Chemical Company Ltd.) following the procedure used in Example 24. Mass spectrum (ES) MH+=492. Conditions: See reaction.notes.procedur...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
c1cscn1.c1ccccc1.C1C[NH]CC[NH]1.C1CC1.c1ccc2c(c1)OCCO2
HBr
null
null
null
N#CN.O=C(CBr)c1ccc2c(c1)OCCO2.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc2c(c1)OCCO2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-00c077eb05ac42d3b480fa4c391efc38
N#CN.O=C(CBr)c1ccc(O)c(F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc(O)c(F)c1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1.BrCC(=O)C1=CC(=C(C=C1)O)F>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)O)F)NC1=CC=C(C=C1)N1CCN(CC1)CC1CC1
[N:1]#[C:2][NH2:3].Br[CH2:23][C:24](=[O:25])[c:26]1[cH:27][cH:28][c:29]([OH:30])[c:31]([F:32])[cH:33]1.[C:4](=[N:5][c:6]1[cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][N:13]([CH2:14][CH:15]3[CH2:16][CH2:17]3)[CH2:18][CH2:19]2)[cH:20][cH:21]1)=[S:22]>>[NH2:1][c:2]1[n:3][c:4]([NH:5][c:6]2[cH:7][cH:8][c:9]([N:10]3[CH2:11][CH2:...
N#CN.O=C(CBr)c1ccc(O)c(F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc(O)c(F)c1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-cyclopropylmethylpiperazine (of Example 14G) and 2-bromo-1-(3-fluoro-4-hydroxyphenyl)ethanone (of Example 14M) following the procedure used in Example 24. Mass spectrum (ES) MH+=468. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
c1cscn1.c1ccccc1.C1C[NH]CC[NH]1.C1CC1.c1ccccc1
HBr
null
null
null
N#CN.O=C(CBr)c1ccc(O)c(F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1ccc(O)c(F)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3cb452d5092d4ae89fecc9ecd25459f7
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1cccc(OC(F)F)c1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(OC(F)F)c4)s3)cc2)CC1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C.BrCC(=O)C1=CC(=CC=C1)OC(F)F>>NC=1N=C(SC1C(=O)C1=CC(=CC=C1)OC(F)F)NC1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:28])[cH:29][cH:30]2)[CH2:31][CH2:32]1.[NH2:12][C:13]#[N:14].Br[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][cH:21][c:22]([O:23][CH:24]([F:25])[F:26])[cH:27]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH:10][c:11]3[n:12][c:13]([NH2...
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1cccc(OC(F)F)c1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(OC(F)F)c4)s3)cc2)CC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-methylpiperazine (of Example 1) and 2-bromo-1-(3-difluoromethoxy-phenyl)ethanone (of Example 14L) following the procedure used in Example 24. Mass spectrum (ES) MH+=460. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1
HBr
null
null
null
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.O=C(CBr)c1cccc(OC(F)F)c1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(OC(F)F)c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-04d595ef5af24223bfc0b9fd7caf593a
N#CN.O=C(CBr)c1cccc(F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1cccc(F)c1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1.BrCC(=O)C1=CC(=CC=C1)F>>NC=1N=C(SC1C(=O)C1=CC(=CC=C1)F)NC1=CC=C(C=C1)N1CCN(CC1)CC1CC1
[N:1]#[C:2][NH2:3].Br[CH2:23][C:24](=[O:25])[c:26]1[cH:27][cH:28][cH:29][c:30]([F:31])[cH:32]1.[C:4](=[N:5][c:6]1[cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][N:13]([CH2:14][CH:15]3[CH2:16][CH2:17]3)[CH2:18][CH2:19]2)[cH:20][cH:21]1)=[S:22]>>[NH2:1][c:2]1[n:3][c:4]([NH:5][c:6]2[cH:7][cH:8][c:9]([N:10]3[CH2:11][CH2:12][N:13...
N#CN.O=C(CBr)c1cccc(F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1cccc(F)c1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatphenyl)-4-cyclopropylmethylpiperazine (of Example 14G) and 2-bromo-1-(3-fluorophenyl)ethanone (Aldrich) following the procedure used in Example 24 Mass spectrum (ES) MH+=452. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
c1cscn1.c1ccccc1.C1C[NH]CC[NH]1.C1CC1.c1ccccc1
HBr
null
null
null
N#CN.O=C(CBr)c1cccc(F)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>Nc1nc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)sc1C(=O)c1cccc(F)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b346d66b2c9c44adaf6cbc93142ddcf2
COc1ccc(C(=O)CBr)cc1F.N#CN.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>COc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(CC5CC5)CC4)cc3)nc2N)cc1F
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1.BrCC(=O)C1=CC(=C(C=C1)OC)F>>NC=1N=C(SC1C(=O)C1=CC(=C(C=C1)OC)F)NC1=CC=C(C=C1)N1CCN(CC1)CC1CC1
Br[CH2:9][C:7]([c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[c:33]([F:34])[cH:32]1)=[O:8].[NH2:29][C:30]#[N:31].[S:10]=[C:11]=[N:12][c:13]1[cH:14][cH:15][c:16]([N:17]2[CH2:18][CH2:19][N:20]([CH2:21][CH:22]3[CH2:23][CH2:24]3)[CH2:25][CH2:26]2)[cH:27][cH:28]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([C:7](=[O:8])[c:9]2[s:10][c:11]([...
COc1ccc(C(=O)CBr)cc1F.N#CN.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
COc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(CC5CC5)CC4)cc3)nc2N)cc1F
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCN(CC4CC4)CC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-cyclopropylmethylpiperazine (of Example 14G) and 2-bromo-1-(3-fluoro-4-methoxyphenyl)ethanone (of Example 13) following the procedure used in Example 24. Mass spectrum (ES) MH+=482. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
c1ccccc1.c1cscn1.c1ccccc1.C1C[NH]CC[NH]1.C1CC1
HBr
null
null
null
COc1ccc(C(=O)CBr)cc1F.N#CN.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>COc1ccc(C(=O)c2sc(Nc3ccc(N4CCN(CC5CC5)CC4)cc3)nc2N)cc1F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-25d1fdad70a740bb8250dd9d84aad07f
N#CN.O=C(CBr)c1cccc(O)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(O)c4)s3)cc2)CC1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)CC1CC1.BrCC(=O)C1=CC(=CC=C1)O>>NC=1N=C(SC1C(=O)C1=CC(=CC=C1)O)NC1=CC=C(C=C1)N1CCN(CC1)C
[NH2:12][C:13]#[N:14].Br[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][cH:21][c:22]([OH:23])[cH:24]1.C1CC1[CH2:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:25])[cH:26][cH:27]2)[CH2:28][CH2:29]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH:10][c:11]3[n:12][c:13]([NH2:14])[c:15]([C:...
N#CN.O=C(CBr)c1cccc(O)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(O)c4)s3)cc2)CC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
afe22251e31860d151b8b251b14d1e16fb67bd2cf918f23bb8a875f5cdf1a9c0
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[C:5]-[#7:6](-[CH2;D2;+0:7]-C1-C-C-1)-[C:8].[S;H0;D1;+0:9]=[C;H0;D2;+0:10]=[N;H0;D2;+0:11]-[c:12](:[c:13]):[c:14].[N;H0;D1;+0:15]#[C;H0;D2;+0:16]-[NH2;D1;+0:17]>>[C:5]-[#7:6](-[CH3;D1;+0:7])-[C:8].[NH2;D1;+0:15]-[c;H0;D3;+0:16]1:[n;H0;D2;+0:17]:[c;H0;D3;+0:10](-[NH;D2;+0:11]-[...
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-cyclopropylmethylpiperazine (of Example 1) and 2-bromo-1-(3-hydroxyphenyl)ethanone (of Example 14N) following the procedure used in Example 24. Mass spectrum (ES) MH+=410. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
C1CC1
c1cscn1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1
HBr
null
null
null
N#CN.O=C(CBr)c1cccc(O)c1.S=C=Nc1ccc(N2CCN(CC3CC3)CC2)cc1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(O)c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c603c17d1e644a2c978edd1e4dbbd2c6
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.N#Cc1cccc(C(=O)CBr)c1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(C#N)c4)s3)cc2)CC1
N#CN.N(=C=S)C1=CC=C(C=C1)N1CCN(CC1)C.C(#N)C=1C=C(C(CBr)=O)C=CC1>>NC=1N=C(SC1C(=O)C=1C=C(C#N)C=CC1)NC1=CC=C(C=C1)N1CCN(CC1)C
[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([N:10]=[C:11]=[S:26])[cH:27][cH:28]2)[CH2:29][CH2:30]1.[NH2:12][C:13]#[N:14].Br[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][cH:21][c:22]([C:23]#[N:24])[cH:25]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[cH:7][cH:8][c:9]([NH:10][c:11]3[n:12][c:13]([NH2:14])[c:15]([C...
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.N#Cc1cccc(C(=O)CBr)c1
CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(C#N)c4)s3)cc2)CC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b99ec609035316c2a2b31cbe39b4884eced779d63c233138f1bb7b0b5332bbd9
f823888efa3dd9a83cac8c606836fbef62e4a8aeb8551af6549e3b12f8a39204
O=C(c1ccccc1)c1cnc(Nc2ccc(N3CCNCC3)cc2)s1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[N;H0;D1;+0:5]#[C;H0;D2;+0:6]-[NH2;D1;+0:7].[S;H0;D1;+0:8]=[C;H0;D2;+0:9]=[N;H0;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[NH2;D1;+0:5]-[c;H0;D3;+0:6]1:[n;H0;D2;+0:7]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[c:11](:[c:12]):[c:13]):[s;H0;D2;+0:8]:[c;H0;D3;+0:1]:1-[C:2](=[O;D1;H0:3])-[c:4]
null
[]
null
null
null
null
This compound was prepared from cyanamide, 1-(4-isothiocyanatophenyl)-4-methylpiperazine (of Example 1) and 3-cyanophenacyl bromide (Maybridge Chemical Co. Ltd.) following the procedure used in Example 24. Mass spectrum (ES) MH+=419. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Cyanamide.Ketone.Isothiocyanate
Ketone.Primary amine.Secondary amine
null
c1cscn1
C1C[NH]CC[NH]1.c1ccccc1.c1cscn1.c1ccccc1
HBr
null
null
null
CN1CCN(c2ccc(N=C=S)cc2)CC1.N#CN.N#Cc1cccc(C(=O)CBr)c1>>CN1CCN(c2ccc(Nc3nc(N)c(C(=O)c4cccc(C#N)c4)s3)cc2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5f7428243e1e42a2ae90f190d4aceb30
CC(=O)NC[C@H]1CN(c2cc(F)c(I)c(F)c2)C(=O)O1.COc1ccc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2F)cn1>>COc1ccc(-c2c(F)cc(N3C[C@H](CNC(C)=O)OC3=O)cc2F)cn1
FC=1C=C(C=C(C1I)F)N1C(O[C@H](C1)CNC(C)=O)=O.FC=1C=C(C=CC1C=1C=NC(=CC1)OC)N1C(O[C@H](C1)CNC(C)=O)=O>>FC=1C=C(C=C(C1C=1C=NC(=CC1)OC)F)N1C(O[C@H](C1)CNC(C)=O)=O
CC(=O)NC[C@H]1CN(c2cc(F)c(I)c([F:9])c2)C(=O)O1.[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][cH:10][c:11]([N:12]3[CH2:13][C@H:14]([CH2:15][NH:16][C:17]([CH3:18])=[O:19])[O:20][C:21]3=[O:22])[cH:23][c:24]2[F:25])[cH:26][n:27]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[c:8]([F:9])[cH:10][c:11]([N:12]3[CH2:13][C@H:...
CC(=O)NC[C@H]1CN(c2cc(F)c(I)c(F)c2)C(=O)O1.COc1ccc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2F)cn1
COc1ccc(-c2c(F)cc(N3C[C@H](CNC(C)=O)OC3=O)cc2F)cn1
null
null
null
Functional Group Interconversion
OtherReaction
d4b5322c27601307394c725f5c94ebd4103ee51f47d69dfacf778281cc0e2eb6
721c7aa90abd60eb14ef592153438764d721e980179827d6757b21b618ed0ef2
O=C1OCCN1c1ccc(-c2cccnc2)cc1
C-C(=O)-N-C-[C@@H]1-C-N(-c2:c:c(-F):c(-I):c(-[F;H0;D1;+0:1]):c:2)-C(=O)-O-1.[#7;a:2]:[c:3]:[c:4]-[c:5](:[c:6]):[cH;D2;+0:7]:[c:8]:[c:9]>>[#7;a:2]:[c:3]:[c:4]-[c:5](:[c:6]):[c;H0;D3;+0:7](-[F;H0;D1;+0:1]):[c:8]:[c:9]
null
[]
null
null
null
null
N-({(5S)-3-[3,5-difluoro-4-(6-methoxypyridin-3-yl)phenyl]-2-oxo-1,3-oxazolidin-5-yl}methyl)acetamide is prepared by the route described in Example 1 substituting N-{[(5S)-3-(3,5-difluoro-4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methyl}acetamide for N-({(5S)-3-[3-fluoro-4-(6-methoxypyridin-3-yl)phenyl]-2-oxo-1,3-oxazolid...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Aromatic halide.Carbamic ester.Ether.Secondary amide
Aromatic halide
C1COCN1.c1ccccc1.c1ccccc1
c1ccccc1
c1ccncc1.c1ccccc1.C1COC[NH]1
HF.I-
null
null
null
CC(=O)NC[C@H]1CN(c2cc(F)c(I)c(F)c2)C(=O)O1.COc1ccc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2F)cn1>>COc1ccc(-c2c(F)cc(N3C[C@H](CNC(C)=O)OC3=O)cc2F)cn1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-481e7c54b6434612a675d5ca6d8123d4
CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1.CC(C)(C)OC(=O)NC[C@H]1CN(c2ccc(I)cc2)C(=O)O1>>CC(=O)NC[C@H]1CN(c2ccc(C3CCC(=O)NC3)cc2)C(=O)O1
IC1=CC=C(C=C1)N1C(O[C@H](C1)CNC(OC(C)(C)C)=O)=O.FC=1C=C(C=CC1I)N1C(O[C@H](C1)CNC(C)=O)=O>>O=C1O[C@H](CN1C1=CC=C(C=C1)C1CNC(CC1)=O)CNC(C)=O
F[c:20]1[c:12](I)[cH:11][cH:10][c:9]([N:8]2[CH2:7][C@H:6]([CH2:5][NH:4][C:2]([CH3:1])=[O:3])[O:24][C:22]2=[O:23])[cH:21]1.CC(C)(C)OC(=O)N[CH2:14][C@@H:13]1O[C:16](=[O:17])[N:18](c2ccc(I)[cH:15]c2)[CH2:19]1>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([CH:13]3[CH2:14][CH2:15][C:16](=...
CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1.CC(C)(C)OC(=O)NC[C@H]1CN(c2ccc(I)cc2)C(=O)O1
CC(=O)NC[C@H]1CN(c2ccc(C3CCC(=O)NC3)cc2)C(=O)O1
null
null
null
C-C Coupling
OtherReaction
59e32096c760eae73ed2de06f4095cf7d765ae537c9f5008658d9e89b5c8e125
e1bea111e0647ea8b1abfb30b0498d8c9c2e13198d7d09566034da932ea95a38
O=C1CCC(c2ccc(N3CCOC3=O)cc2)CN1
C-C(-C)(-C)-O-C(=O)-N-[CH2;D2;+0:1]-[C@@H;D3;+0:2]1-O-[C;H0;D3;+0:3](=[O;D1;H0:4])-[N;H0;D3;+0:5](-c2:c:[cH;D2;+0:6]:c(-I):c:c:2)-[C:7]-1.F-[c;H0;D3;+0:8]1:[c:9]:[c:10]:[c:11]:[c:12]:[c;H0;D3;+0:13]:1-I>>[O;D1;H0:4]=[C;H0;D3;+0:3]1-[CH2;D2;+0:6]-[CH2;D2;+0:1]-[CH;D3;+0:2](-[c;H0;D3;+0:13]2:[c:12]:[c:11]:[c:10]:[c:9]:[c...
null
[]
null
null
null
null
N-({(5S)-2-oxo-3-[4-(6-oxopiperidin-3-yl)phenyl]-1,3-oxazolidin-5-yl}methyl)acetamide is prepared by the route described in Example 1 substituting tert-butyl [(5S)-3-(4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methylcarbamate for N-{[(5S)-(3-fluoro-4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methyl}acetamide. 1H-NMR (DMSO) δ:...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Aromatic halide.Carbamic ester.Carbamic ester.Ether.Ether.Boc
Secondary amide
c1ccccc1.C1COC[NH]1.c1ccccc1
c1ccccc1.C1CCNCC1
C1COC[NH]1.c1ccccc1.C1CCNCC1
HF.I-
null
null
null
CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1.CC(C)(C)OC(=O)NC[C@H]1CN(c2ccc(I)cc2)C(=O)O1>>CC(=O)NC[C@H]1CN(c2ccc(C3CCC(=O)NC3)cc2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b8b7a9a119eb41aeb93ede6115a10d01
CI.COc1ccc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2)cn1>>CC(=O)NC[C@H]1CN(c2ccc(-c3ccc(=O)n(C)c3)cc2)C(=O)O1
C1CCOC1.COC1=CC=C(C=N1)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O.C([O-])([O-])=O.[K+].[K+].CI>>CN1C=C(C=CC1=O)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O
I[CH3:19].C[O:17][c:16]1[cH:15][cH:14][c:13](-[c:12]2[cH:11][cH:10][c:9]([N:8]3[CH2:7][C@H:6]([CH2:5][NH:4][C:2]([CH3:1])=[O:3])[O:25][C:23]3=[O:24])[cH:22][cH:21]2)[cH:20][n:18]1>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12](-[c:13]3[cH:14][cH:15][c:16](=[O:17])[n:18]([CH3:19])[cH:2...
CI.COc1ccc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2)cn1
CC(=O)NC[C@H]1CN(c2ccc(-c3ccc(=O)n(C)c3)cc2)C(=O)O1
null
null
C(Cl)Cl
Acylation
OtherReaction
545dd64706b916c5c1e0993ccc3faf9b2ae2a984dff2896afa16f308b6704fa2
44ce3ef111697e4edd80a3a62efdfdfb9c6acd9c324ef9a7c10ca658a5992f13
O=C1OCCN1c1ccc(-c2ccc(=O)[nH]c2)cc1
C-[O;H0;D2;+0:1]-[c;H0;D3;+0:2]1:[c:3]:[c:4]:[c:5]:[c:6]:[n;H0;D2;+0:7]:1.I-[CH3;D1;+0:8]>>[CH3;D1;+0:8]-[n;H0;D3;+0:7]1:[c:6]:[c:5]:[c:4]:[c:3]:[c;H0;D3;+0:2]:1=[O;H0;D1;+0:1]
53
[{"value": 53.0, "product": "CN1C=C(C=CC1=O)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
To a stirred anhydrous THF (10 mL) mixture of N-({(5S)-3-[4-(6-methoxypyridin-3-yl)phenyl]-2-oxo-1,3-oxazolidin-5-yl}methyl)acetamide (0.10 g, 0.29 mmol) in a sealed tube, is added potassium carbonate (0.04 g, 0.58 mmol) and methyl iodide (0.1 mL, 1.7 mmol). The mixture is heated to 85° C. for 16 hours. The reaction is...
10.6084/m9.figshare.5104873.v1
null
Ether
null
c1ccncc1
c1ccncc1
C1COC[NH]1.c1ccccc1.c1ccncc1
HI
C(Cl)Cl
85
null
CI.COc1ccc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2)cn1>C(Cl)Cl>CC(=O)NC[C@H]1CN(c2ccc(-c3ccc(=O)n(C)c3)cc2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5c6bb1e0d3264955b588e9c074389bb6
CC(=O)NC[C@H]1CN(c2ccc(-c3ccc(=O)n(C)c3)cc2)C(=O)O1>>CC(=O)NC[C@H]1CN(c2ccc(C3CCC(=O)N(C)C3)cc2)C(=O)O1
CN1C=C(C=CC1=O)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O>>CN1CC(CCC1=O)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O
[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12](-[c:13]3[cH:14][cH:15][c:16](=[O:17])[n:18]([CH3:19])[cH:20]3)[cH:21][cH:22]2)[C:23](=[O:24])[O:25]1>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([CH:13]3[CH2:14][CH2:15][C:16](=[O:17])[N:18]([CH3:19])[...
CC(=O)NC[C@H]1CN(c2ccc(-c3ccc(=O)n(C)c3)cc2)C(=O)O1
CC(=O)NC[C@H]1CN(c2ccc(C3CCC(=O)N(C)C3)cc2)C(=O)O1
null
[Pd]
CO
Reduction
OtherReaction
c3195e041c676c98fe57174265b77b3d65854f9e1e38d3c19cbfffe2c63e429c
a9abb915c2e8fb5c88d9357a865a3b933b515d3da17c0f40274f1e391bda35ae
O=C1CCC(c2ccc(N3CCOC3=O)cc2)CN1
[C;D1;H3:1]-[n;H0;D3;+0:2]1:[cH;D2;+0:3]:[c;H0;D3;+0:4](-[c;H0;D3;+0:5](:[c:6]:[c:7]):[c:8]:[c:9]):[cH;D2;+0:10]:[cH;D2;+0:11]:[c;H0;D3;+0:12]:1=[O;D1;H0:13]>>[C;D1;H3:1]-[N;H0;D3;+0:2]1-[CH2;D2;+0:3]-[CH;D3;+0:4](-[c;H0;D3;+0:5](:[c:6]:[c:7]):[c:8]:[c:9])-[CH2;D2;+0:10]-[CH2;D2;+0:11]-[C;H0;D3;+0:12]-1=[O;D1;H0:13]
97.4
[{"value": 96.0, "product": "CN1CC(CCC1=O)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.4, "product": "CN1CC(CCC1=O)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a mixture of N-({(5S)-3-[4-(1-methyl-6-oxo-1,6-dihydropyridin-3-yl)phenyl]-2-oxo-1,3-oxazolidin-5-yl}methyl)acetamide (0.179 g. 0.52 mmol) in 20 mL of MeOH is added 0.05 g of 10% palladium on activated charcoal. The mixture is hydrogenated at 50 psi for 16 hours. The reaction mixture is filtered through celite, sili...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amide
c1ccncc1
C1CC[NH]CC1
C1COC[NH]1.c1ccccc1.C1CC[NH]CC1
null
[Pd].CO
null
16
CC(=O)NC[C@H]1CN(c2ccc(-c3ccc(=O)n(C)c3)cc2)C(=O)O1>[Pd].CO>CC(=O)NC[C@H]1CN(c2ccc(C3CCC(=O)N(C)C3)cc2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f5a70fb75d8f4ab78c65ac2e0f2a45cd
CC(=O)NC[C@H]1CN(c2cc(F)c(I)c(F)c2)C(=O)O1.CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1>>CC(=O)NC[C@H]1CN(c2cc(F)c(C3CCNC(=O)C3)c(F)c2)C(=O)O1
FC=1C=C(C=C(C1I)F)N1C(O[C@H](C1)CNC(C)=O)=O.FC=1C=C(C=CC1I)N1C(O[C@H](C1)CNC(C)=O)=O>>FC=1C=C(C=C(C1C1CC(NCC1)=O)F)N1C(O[C@H](C1)CNC(C)=O)=O
I[c:13]1[c:11]([F:12])[cH:10][c:9]([N:8]2[CH2:7][C@H:6]([CH2:5][NH:4][C:2]([CH3:1])=[O:3])[O:26][C:24]2=[O:25])[cH:23][c:21]1[F:22].O=C1O[C@@H]([CH2:16][NH:17][C:18](=[O:19])[CH3:20])CN1c1cc(F)[c:14](I)[cH:15]c1>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][c:11]([F:12])[c:13]([CH:14]3[CH2:15][CH...
CC(=O)NC[C@H]1CN(c2cc(F)c(I)c(F)c2)C(=O)O1.CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1
CC(=O)NC[C@H]1CN(c2cc(F)c(C3CCNC(=O)C3)c(F)c2)C(=O)O1
null
null
null
C-C Coupling
OtherReaction
9848f145d33a3b77976f5af411dab89172424ee5e8c4f6ad59dcb6388908519f
8f99d3d6d09d378cd3451a4aabedce8298e57da208307a564bd3a9b8c5a1a312
O=C1CC(c2ccc(N3CCOC3=O)cc2)CCN1
F-c1:c:c(-N2-C-[C@@H](-[CH2;D2;+0:1]-[#7:2]-[C:3](-[CH3;D1;+0:4])=[O;D1;H0:5])-O-C-2=O):c:[cH;D2;+0:6]:[c;H0;D3;+0:7]:1-I.I-[c;H0;D3;+0:8](:[c:9](-[F;D1;H0:10]):[c:11]):[c:12](-[F;D1;H0:13]):[c:14]>>[F;D1;H0:10]-[c:9](:[c:11]):[c;H0;D3;+0:8](-[CH;D3;+0:7]1-[CH2;D2;+0:6]-[CH2;D2;+0:1]-[#7:2]-[C:3](=[O;D1;H0:5])-[CH2;D2;...
null
[]
null
null
null
null
N-({(5S)-3-[3,5-difluoro-4-(2-oxopiperidin-4-yl)phenyl]-2-oxo-1,3-oxazolidin-5-yl}methyl)acetamide is prepared as in the route described in Example 16 substituting N-{[(5S)-3-(3,5-difluoro-4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methyl}acetamide for 1 N-{[(5S)-3-(3-fluoro-4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methyl}...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Aromatic halide.Carbamic ester.Ether
null
c1ccccc1.C1COCN1.c1ccccc1
c1ccccc1.C1CCNCC1
C1COC[NH]1.c1ccccc1.C1CCNCC1
HF.I-
null
null
null
CC(=O)NC[C@H]1CN(c2cc(F)c(I)c(F)c2)C(=O)O1.CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1>>CC(=O)NC[C@H]1CN(c2cc(F)c(C3CCNC(=O)C3)c(F)c2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-603ab36590b94febb01366d65d2beff1
CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1.CC(C)(C)OC(=O)NC[C@H]1CN(c2ccc(I)cc2)C(=O)O1>>CC(=O)NC[C@H]1CN(c2ccc(C3CCNC(=O)C3)cc2)C(=O)O1
IC1=CC=C(C=C1)N1C(O[C@H](C1)CNC(OC(C)(C)C)=O)=O.FC=1C=C(C=CC1I)N1C(O[C@H](C1)CNC(C)=O)=O>>O=C1O[C@H](CN1C1=CC=C(C=C1)C1CC(NCC1)=O)CNC(C)=O
F[c:20]1[c:12](I)[cH:11][cH:10][c:9]([N:8]2[CH2:7][C@H:6]([CH2:5][NH:4][C:2]([CH3:1])=[O:3])[O:24][C:22]2=[O:23])[cH:21]1.CC(C)(C)O[C:17]([NH:16][CH2:15][C@H:14]1CN(c2cc[c:13](I)[cH:19]c2)C(=O)O1)=[O:18]>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([CH:13]3[CH2:14][CH2:15][NH:16][C:...
CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1.CC(C)(C)OC(=O)NC[C@H]1CN(c2ccc(I)cc2)C(=O)O1
CC(=O)NC[C@H]1CN(c2ccc(C3CCNC(=O)C3)cc2)C(=O)O1
null
null
null
C-C Coupling
OtherReaction
5d72289eadb17142a403fba2d58f954256fd4195024b0107234b1eac52ee5906
e1bea111e0647ea8b1abfb30b0498d8c9c2e13198d7d09566034da932ea95a38
O=C1CC(c2ccc(N3CCOC3=O)cc2)CCN1
C-C(-C)(-C)-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3]-[C:4]-[C@H;D3;+0:5]1-C-N(-c2:c:[cH;D2;+0:6]:[c;H0;D3;+0:7](-I):c:c:2)-C(=O)-O-1.F-[c;H0;D3;+0:8]1:[c:9]:[c:10]:[c:11]:[c:12]:[c;H0;D3;+0:13]:1-I>>[O;D1;H0:2]=[C;H0;D3;+0:1]1-[#7:3]-[C:4]-[CH2;D2;+0:5]-[CH;D3;+0:7](-[c;H0;D3;+0:13]2:[c:12]:[c:11]:[c:10]:[c:9]:[cH;D2;+0:8...
null
[]
null
null
null
null
N-({(5S)-2-oxo-3-[4-(2-oxopiperidin-4-yl)phenyl]-1,3-oxazolidin-5-yl}methyl)acetamide is prepared as described in the route described in Example 16 substituting tert-butyl [(5S)-3-(4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methylcarbamate for N-{[(5S)-3-(3-fluoro-4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methyl}acetamide. ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Aromatic halide.Carbamic ester.Carbamic ester.Ether.Ether.Boc
Secondary amide
c1ccccc1.C1COCN1.c1ccccc1
c1ccccc1.C1CCNCC1
C1COC[NH]1.c1ccccc1.C1CCNCC1
HF.I-
null
null
null
CC(=O)NC[C@H]1CN(c2ccc(I)c(F)c2)C(=O)O1.CC(C)(C)OC(=O)NC[C@H]1CN(c2ccc(I)cc2)C(=O)O1>>CC(=O)NC[C@H]1CN(c2ccc(C3CCNC(=O)C3)cc2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-68f084637a2845fca977375ed451ee03
CI.COc1cc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2)ccn1>>CC(=O)NC[C@H]1CN(c2ccc(-c3ccn(C)c(=O)c3)cc2)C(=O)O1
C1CCOC1.COC1=NC=CC(=C1)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O.C([O-])([O-])=O.[K+].[K+].CI>>CN1C(C=C(C=C1)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O)=O
I[CH3:17].C[O:19][c:18]1[n:16][cH:15][cH:14][c:13](-[c:12]2[cH:11][cH:10][c:9]([N:8]3[CH2:7][C@H:6]([CH2:5][NH:4][C:2]([CH3:1])=[O:3])[O:25][C:23]3=[O:24])[cH:22][cH:21]2)[cH:20]1>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12](-[c:13]3[cH:14][cH:15][n:16]([CH3:17])[c:18](=[O:19])[cH:2...
CI.COc1cc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2)ccn1
CC(=O)NC[C@H]1CN(c2ccc(-c3ccn(C)c(=O)c3)cc2)C(=O)O1
null
null
C(Cl)Cl
Acylation
OtherReaction
545dd64706b916c5c1e0993ccc3faf9b2ae2a984dff2896afa16f308b6704fa2
44ce3ef111697e4edd80a3a62efdfdfb9c6acd9c324ef9a7c10ca658a5992f13
O=C1OCCN1c1ccc(-c2cc[nH]c(=O)c2)cc1
C-[O;H0;D2;+0:1]-[c;H0;D3;+0:2]1:[c:3]:[c:4]:[c:5]:[c:6]:[n;H0;D2;+0:7]:1.I-[CH3;D1;+0:8]>>[CH3;D1;+0:8]-[n;H0;D3;+0:7]1:[c:6]:[c:5]:[c:4]:[c:3]:[c;H0;D3;+0:2]:1=[O;H0;D1;+0:1]
69
[{"value": 69.0, "product": "CN1C(C=C(C=C1)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
To a stirred anhydrous THF (10 mL) mixture of N-({(5S)-3-[4-(2-methoxypyridin-4-yl)phenyl]-2-oxo-1,3-oxazolidin-5-yl}methyl)acetamide (0.667 g, 1.95 mmol) in a sealed tube, is added potassium carbonate (0.807 g, 6.0 mmol) and methyl iodide (1 mL, 17 mmol). The mixture is heated to 85° C. for 16 hours. The reaction is c...
10.6084/m9.figshare.5104873.v1
null
Ether
null
c1ccncc1
c1ccncc1
C1COC[NH]1.c1ccccc1.c1ccncc1
HI
C(Cl)Cl
85
null
CI.COc1cc(-c2ccc(N3C[C@H](CNC(C)=O)OC3=O)cc2)ccn1>C(Cl)Cl>CC(=O)NC[C@H]1CN(c2ccc(-c3ccn(C)c(=O)c3)cc2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-aafc07e1d0ec45f3bf9d814970cd12ea
CC(=O)NC[C@H]1CN(c2ccc(-c3ccn(C)c(=O)c3)cc2)C(=O)O1>>CC(=O)NC[C@H]1CN(c2ccc(C3CCN(C)C(=O)C3)cc2)C(=O)O1
CN1C(C=C(C=C1)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O)=O>>CN1C(CC(CC1)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O)=O
[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12](-[c:13]3[cH:14][cH:15][n:16]([CH3:17])[c:18](=[O:19])[cH:20]3)[cH:21][cH:22]2)[C:23](=[O:24])[O:25]1>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][C@H:6]1[CH2:7][N:8]([c:9]2[cH:10][cH:11][c:12]([CH:13]3[CH2:14][CH2:15][N:16]([CH3:17])[C:18](=[O:19])[...
CC(=O)NC[C@H]1CN(c2ccc(-c3ccn(C)c(=O)c3)cc2)C(=O)O1
CC(=O)NC[C@H]1CN(c2ccc(C3CCN(C)C(=O)C3)cc2)C(=O)O1
null
[Pd]
CO
Reduction
OtherReaction
c3195e041c676c98fe57174265b77b3d65854f9e1e38d3c19cbfffe2c63e429c
a9abb915c2e8fb5c88d9357a865a3b933b515d3da17c0f40274f1e391bda35ae
O=C1CC(c2ccc(N3CCOC3=O)cc2)CCN1
[C;D1;H3:1]-[n;H0;D3;+0:2]1:[cH;D2;+0:3]:[cH;D2;+0:4]:[c;H0;D3;+0:5](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[cH;D2;+0:11]:[c;H0;D3;+0:12]:1=[O;D1;H0:13]>>[C;D1;H3:1]-[N;H0;D3;+0:2]1-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[CH;D3;+0:5](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10])-[CH2;D2;+0:11]-[C;H0;D3;+0:12]-1=[O;D1;H0:13]
97.5
[{"value": 96.0, "product": "CN1C(CC(CC1)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.5, "product": "CN1C(CC(CC1)C1=CC=C(C=C1)N1C(O[C@H](C1)CNC(C)=O)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a mixture of N-({(5S)-3-[4-(1-methyl-2-oxo-1,2-dihydropyridin-4-yl)phenyl]-2-oxo-1,3-oxazolidin-5-yl}methyl)acetamide (0.170 g. 0.49 mmol) in 20 mL of MeOH is added 0.05 g of 10% palladium on activated charcoal. The mixture is hydrogenated at 50 psi for 16 hours. The reaction mixture is filtered through celite, sili...
10.6084/m9.figshare.5104873.v1
null
null
Tertiary amide
c1ccncc1
C1CC[NH]CC1
C1COC[NH]1.c1ccccc1.C1CC[NH]CC1
null
[Pd].CO
null
16
CC(=O)NC[C@H]1CN(c2ccc(-c3ccn(C)c(=O)c3)cc2)C(=O)O1>[Pd].CO>CC(=O)NC[C@H]1CN(c2ccc(C3CCN(C)C(=O)C3)cc2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-38f98b5e5d954dd4aefeef4cc01d73b6
Cc1ccc(S(=O)(=O)N/N=C/C(Cl)Cl)cc1.NC[C@H]1CN(c2cc(F)c(C3CCC(=O)NC3)c(F)c2)C(=O)O1>>O=C1CCC(c2c(F)cc(N3C[C@H](Cn4ccnn4)OC3=O)cc2F)CN1
NC[C@H]1CN(C(O1)=O)C1=CC(=C(C(=C1)F)C1CCC(NC1)=O)F.FC=1C=C(C=C(C1I)F)N1C(O[C@H](C1)CNC(C)=O)=O.CCN(CC)CC.ClC(\C=N\NS(=O)(=O)C1=CC=C(C=C1)C)Cl>>FC1=C(C(=CC(=C1)N1C(O[C@H](C1)CN1N=NC=C1)=O)F)C1CCC(NC1)=O
Cc1ccc(S(=O)(=O)[NH:19]/[N:18]=[CH:17]/[CH:16](Cl)Cl)cc1.[O:1]=[C:2]1[CH2:3][CH2:4][CH:5]([c:6]2[c:7]([F:8])[cH:9][c:10]([N:11]3[CH2:12][C@H:13]([CH2:14][NH2:15])[O:20][C:21]3=[O:22])[cH:23][c:24]2[F:25])[CH2:26][NH:27]1>>[O:1]=[C:2]1[CH2:3][CH2:4][CH:5]([c:6]2[c:7]([F:8])[cH:9][c:10]([N:11]3[CH2:12][C@H:13]([CH2:14][n...
Cc1ccc(S(=O)(=O)N/N=C/C(Cl)Cl)cc1.NC[C@H]1CN(c2cc(F)c(C3CCC(=O)NC3)c(F)c2)C(=O)O1
O=C1CCC(c2c(F)cc(N3C[C@H](Cn4ccnn4)OC3=O)cc2F)CN1
null
null
CO
Functional Group Interconversion
OtherReaction
5075942d1c359ffbea0abc7bda1d363acb35365d84e84d19f453041d6c512a7e
642892d0a5f6fd725597bcb867e2f43b9086bb600d415ccf63e67d9536d6e549
O=C1CCC(c2ccc(N3C[C@H](Cn4ccnn4)OC3=O)cc2)CN1
C-c1:c:c:c(-S(=O)(=O)-[NH;D2;+0:1]/[N;H0;D2;+0:2]=[CH;D2;+0:3]/[CH;D3;+0:4](-Cl)-Cl):c:c:1.[#8:5]-[C:6]-[C:7]-[NH2;D1;+0:8]>>[#8:5]-[C:6]-[C:7]-[n;H0;D3;+0:8]1:[cH;D2;+0:4]:[cH;D2;+0:3]:[n;H0;D2;+0:2]:[n;H0;D2;+0:1]:1
null
[]
null
null
16
HOUR
5-{4-[(5S)-5-(aminomethyl)-2-oxo-1,3-oxazolidin-3-yl]-2,6-difluorophenyl}piperidin-2-one (0.1 g, 0.31 mmol) (prepared by the route described in Example 1, substituting N-{[(5S)-3-(3,5-difluoro-4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methyl}acetamide) is dissolved in MeOH (2 mL). To this mixture is added Et3N (0.125 ml,...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Hydrazone.Tosylate.Secondary halide.Secondary halide.Primary amine
null
c1ccccc1
c1c[nH]nn1
C1CCNCC1.c1ccccc1.C1COC[NH]1.c1c[nH]nn1
TsOH.HCl
CO
null
16
Cc1ccc(S(=O)(=O)N/N=C/C(Cl)Cl)cc1.NC[C@H]1CN(c2cc(F)c(C3CCC(=O)NC3)c(F)c2)C(=O)O1>CO>O=C1CCC(c2c(F)cc(N3C[C@H](Cn4ccnn4)OC3=O)cc2F)CN1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8ef35b9c9c5c40bcabb7b408e1cb86f0
C1CCNC1.COC(=O)CC(C)=O>>COC(=O)C=C(C)C1CCCN1
C(CC(=O)C)(=O)OC.N1CCCC1>>N1C(CCC1)C(=CC(=O)OC)C
[CH2:8]1[CH2:9][CH2:10][CH2:11][NH:12]1.O=[C:6]([CH2:5][C:3]([O:2][CH3:1])=[O:4])[CH3:7]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]=[C:6]([CH3:7])[CH:8]1[CH2:9][CH2:10][CH2:11][NH:12]1
C1CCNC1.COC(=O)CC(C)=O
COC(=O)C=C(C)C1CCCN1
null
O.C1(=CC=C(C=C1)S(=O)(=O)O)C
C1(=CC=CC=C1)C
C-C Coupling
OtherReaction
8660069fb91e5b1c8f8d2e6b91aa0e7d72f23b0e3df16a0b8c6114590ddc28ad
79a946b42eb7e7aee42e09efe41630192c1745e07085cd7f7f88cc7b599f9082
C1CCNC1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH2;D2;+0:3]-[C:4](=[O;D1;H0:5])-[#8:6]-[C;D1;H3:7].[#7:8]1-[C:9]-[C:10]-[C:11]-[CH2;D2;+0:12]-1>>[C;D1;H3:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[CH;D2;+0:3]=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:12]1-[#7:8]-[C:9]-[C:10]-[C:11]-1
99.5
[{"value": 99.0, "product": "N1C(CCC1)C(=CC(=O)OC)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.5, "product": "N1C(CCC1)C(=CC(=O)OC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
140
CELSIUS
null
null
Methyl acetoacetate (20 g, 172.23 mmol) was dissolved in 250 mL of toluene, and then pyrrolidine (43 ml, 516.70 mmol) and p-toluenesulfonic acid hydrate (about 100 mg) were added dropwise. After installing a Dean-Stark separator to the reactor, the reaction mixture was refluxed 140° C. for two days, and then solvent wa...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester
Ester
C1CCNC1
C1CCNC1
C1CCNC1
HO-
O.C1(=CC=C(C=C1)S(=O)(=O)O)C.C1(=CC=CC=C1)C
140
null
C1CCNC1.COC(=O)CC(C)=O>O.C1(=CC=C(C=C1)S(=O)(=O)O)C.C1(=CC=CC=C1)C>COC(=O)C=C(C)C1CCCN1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c4f6c0a039404fa9b84557e51bc4c6bf
C1CCNC1.CCOC(=O)CC(C)=O>>CCOC(=O)C=C(C)C1CCCN1
C(CC(=O)C)(=O)OCC.N1CCCC1>>N1C(CCC1)C(=CC(=O)OCC)C
[CH2:9]1[CH2:10][CH2:11][CH2:12][NH:13]1.O=[C:7]([CH2:6][C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH3:8]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]=[C:7]([CH3:8])[CH:9]1[CH2:10][CH2:11][CH2:12][NH:13]1
C1CCNC1.CCOC(=O)CC(C)=O
CCOC(=O)C=C(C)C1CCCN1
null
null
null
C-C Coupling
OtherReaction
8660069fb91e5b1c8f8d2e6b91aa0e7d72f23b0e3df16a0b8c6114590ddc28ad
79a946b42eb7e7aee42e09efe41630192c1745e07085cd7f7f88cc7b599f9082
C1CCNC1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH2;D2;+0:3]-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7].[#7:8]1-[C:9]-[C:10]-[C:11]-[CH2;D2;+0:12]-1>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[CH;D2;+0:3]=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:12]1-[#7:8]-[C:9]-[C:10]-[C:11]-1
null
[]
null
null
null
null
Ethyl 3-tetrahydropyrrolyl-2-butenoate was prepared (21 g, 99%) from ethyl acetoacetate (15.0 g, 115.26 mmol) and pyrrolidine (71.1 mL, 345.78 mmol) in the same manner as described in the above Example 1 (1), and the obtained product was identified with the following NMR data. Conditions: See reaction.notes.procedure_d...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester
Ester
C1CCNC1
C1CCNC1
C1CCNC1
HO-
null
null
null
C1CCNC1.CCOC(=O)CC(C)=O>>CCOC(=O)C=C(C)C1CCCN1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b23c8ba54c484e1bafaf208e0e2e4633
C1CCNC1.C=CCOC(=O)CC(C)=O>>C=CCOC(=O)C=C(C)C1CCCN1
C(CC(=O)C)(=O)OCC=C.N1CCCC1>>N1C(CCC1)C(=CC(=O)OCC=C)C
[CH2:10]1[CH2:11][CH2:12][CH2:13][NH:14]1.O=[C:8]([CH2:7][C:5]([O:4][CH2:3][CH:2]=[CH2:1])=[O:6])[CH3:9]>>[CH2:1]=[CH:2][CH2:3][O:4][C:5](=[O:6])[CH:7]=[C:8]([CH3:9])[CH:10]1[CH2:11][CH2:12][CH2:13][NH:14]1
C1CCNC1.C=CCOC(=O)CC(C)=O
C=CCOC(=O)C=C(C)C1CCCN1
null
null
null
C-C Coupling
OtherReaction
8660069fb91e5b1c8f8d2e6b91aa0e7d72f23b0e3df16a0b8c6114590ddc28ad
79a946b42eb7e7aee42e09efe41630192c1745e07085cd7f7f88cc7b599f9082
C1CCNC1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH2;D2;+0:3]-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7]-[C:8]=[C;D1;H2:9].[#7:10]1-[C:11]-[C:12]-[C:13]-[CH2;D2;+0:14]-1>>[C;D1;H2:9]=[C:8]-[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[CH;D2;+0:3]=[C;H0;D3;+0:1](-[C;D1;H3:2])-[CH;D3;+0:14]1-[#7:10]-[C:11]-[C:12]-[C:13]-1
null
[]
null
null
null
null
Allyl 3-tetrahydropyrrolyl-2-butenoate was prepared (4.7 g, 68%) in the same manner as described in the above Example 1 (1) from allyl acetoacetate (5.0 g, 35.17 mmol) and pyrrolidine (8.8 mL, 105.51 mmol), and the obtained product was identified with the following 1H NMR data. Conditions: See reaction.notes.procedure_...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester
Ester
C1CCNC1
C1CCNC1
C1CCNC1
HO-
null
null
null
C1CCNC1.C=CCOC(=O)CC(C)=O>>C=CCOC(=O)C=C(C)C1CCCN1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-96ae0b4ef29e47f48fb533915a460abe
COC(=O)C=C(C)C1CCCN1.O.O=C1c2ccccc2C(=O)N1CBr>>COC(=O)C(CN1C(=O)c2ccccc2C1=O)C(C)=O
N1C(CCC1)C(=CC(=O)OC)C.BrCN1C(C=2C(C1=O)=CC=CC2)=O.Cl.O>>C1(C=2C(C(N1CC(C(=O)OC)C(C)=O)=O)=CC=CC2)=O
C1CNC([C:18](=[CH:5][C:3]([O:2][CH3:1])=[O:4])[CH3:19])C1.[OH2:20].Br[CH2:6][N:7]1[C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[C:16]1=[O:17]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][N:7]1[C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[C:16]1=[O:17])[C:18]([CH3:19])=[O:20]
COC(=O)C=C(C)C1CCCN1.O.O=C1c2ccccc2C(=O)N1CBr
COC(=O)C(CN1C(=O)c2ccccc2C1=O)C(C)=O
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
0dc29a751f8e39c42176c69c70cd6d74b167d123f582ba8e6e42b4cfcf20a324
e7542302dea48a79cdeb319bd616ca61700e1eb51eca81328aa5c73cb500b762
O=C1NC(=O)c2ccccc21
Br-[CH2;D2;+0:1]-[#7:2]1-[C:3](=[O;D1;H0:4])-[c:5]:[c:6]-[C:7]-1=[O;D1;H0:8].[C;D1;H3:9]-[C;H0;D3;+0:10](=[CH;D2;+0:11]-[C:12](=[O;D1;H0:13])-[#8:14]-[C;D1;H3:15])-C1-C-C-C-N-1.[OH2;D0;+0:16]>>[C;D1;H3:9]-[C;H0;D3;+0:10](=[O;H0;D1;+0:16])-[CH;D3;+0:11](-[CH2;D2;+0:1]-[#7:2]1-[C:3](=[O;D1;H0:4])-[c:5]:[c:6]-[C:7]-1=[O;D...
68
[{"value": 68.0, "product": "C1(C=2C(C(N1CC(C(=O)OC)C(C)=O)=O)=CC=CC2)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
Methyl 3-tetrahydropyrrolyl-2-butenoate (29.0 g, 171.3 mmol) and N-(bromomethyl)phthalimide (43 g, 179.91 mmol) were dissolved in 250 ml of dimethylformamide, and the resulting mixture was then stirred at room temperature for 16 hours under a nitrogen atmosphere. After checking completion of the reaction with TLC, 1N H...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Substituted dicarboximide.Secondary amine
Ketone.Ester.Substituted dicarboximide
C1CCNC1
null
c1ccc2c(c1)C[NH]C2
HBr
CN(C=O)C
null
16
COC(=O)C=C(C)C1CCCN1.O.O=C1c2ccccc2C(=O)N1CBr>CN(C=O)C>COC(=O)C(CN1C(=O)c2ccccc2C1=O)C(C)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-beaa02d0a3f34642896af054ec129f95
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c(F)cccc21>>COC(=O)C(CN1C(=O)c2cccc(F)c2C1=O)C1(C)OCCO1
NCC(C(=O)OC)C1(OCCO1)C.FC1=C2C(C(=O)OC2=O)=CC=C1>>FC1=C2C(N(C(C2=CC=C1)=O)CC(C(=O)OC)C1(OCCO1)C)=O
[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][NH2:7])[C:19]1([CH3:20])[O:21][CH2:22][CH2:23][O:24]1.O1[C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([F:15])[c:16]2[C:17]1=[O:18]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][N:7]1[C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([F:15])[c:16]2[C:17]1=[O:18])[C:19]1([CH3:20])[O:21][...
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c(F)cccc21
COC(=O)C(CN1C(=O)c2cccc(F)c2C1=O)C1(C)OCCO1
null
null
null
Acylation
Phthalic anhydride to phthalimide
c3c986d6e09320348d40a4a59ca107882ce771f249842049dc55e55f334c675b
2bbbf7b24648445e31d33a2a26f8618c2067bd23957587cc459f3c45a03ed48a
O=C1c2ccccc2C(=O)N1CCC1OCCO1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[NH2;D1;+0:6].[O;D1;H0:7]=[C;H0;D3;+0:8]1-O-[C;H0;D3;+0:9](=[O;D1;H0:10])-[c:11](:[c:12]):[c:13]-1:[c:14]>>[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[N;H0;D3;+0:6]1-[C;H0;D3;+0:8](=[O;D1;H0:7])-[c:13](:[c:14]):[c:11](:[c:12])-[C;H0;D3;+0:9]-1=[O;D1;H0:10]
null
[]
null
null
null
null
Methyl 3-(4-fluoro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate was prepared (0.24 g, 28%) in the same manner as described in the above example 5 (1) from methyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (0.50 g, 2.64 mmol) and 3-fluorophthalic anhydride (0.57 g, 3.43 mmol), an...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Ester.Ester.Primary amine
Substituted dicarboximide
c1ccc2c(c1)COC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2.C1COCO1
HO-
null
null
null
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c(F)cccc21>>COC(=O)C(CN1C(=O)c2cccc(F)c2C1=O)C1(C)OCCO1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-55e268810b43421a99d2245b5297b31f
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c(F)ccc(F)c21>>COC(=O)C(CN1C(=O)c2c(F)ccc(F)c2C1=O)C1(C)OCCO1
O=C1N(C(C=2CCCCC12)=O)CC(C(=O)OC)C1(OCCO1)C.NCC(C(=O)OC)C1(OCCO1)C.FC1=C2C(C(=O)OC2=O)=C(C=C1)F>>FC1=C2C(N(C(C2=C(C=C1)F)=O)CC(C(=O)OC)C1(OCCO1)C)=O
[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][NH2:7])[C:20]1([CH3:21])[O:22][CH2:23][CH2:24][O:25]1.O1[C:8](=[O:9])[c:10]2[c:11]([F:12])[cH:13][cH:14][c:15]([F:16])[c:17]2[C:18]1=[O:19]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][N:7]1[C:8](=[O:9])[c:10]2[c:11]([F:12])[cH:13][cH:14][c:15]([F:16])[c:17]2[C:18]1=[O:19])[C:20]1([C...
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c(F)ccc(F)c21
COC(=O)C(CN1C(=O)c2c(F)ccc(F)c2C1=O)C1(C)OCCO1
null
null
null
Acylation
Phthalic anhydride to phthalimide
c3c986d6e09320348d40a4a59ca107882ce771f249842049dc55e55f334c675b
2bbbf7b24648445e31d33a2a26f8618c2067bd23957587cc459f3c45a03ed48a
O=C1c2ccccc2C(=O)N1CCC1OCCO1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[NH2;D1;+0:6].[O;D1;H0:7]=[C;H0;D3;+0:8]1-O-[C;H0;D3;+0:9](=[O;D1;H0:10])-[c:11](:[c:12]):[c:13]-1:[c:14]>>[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[N;H0;D3;+0:6]1-[C;H0;D3;+0:8](=[O;D1;H0:7])-[c:13](:[c:14]):[c:11](:[c:12])-[C;H0;D3;+0:9]-1=[O;D1;H0:10]
null
[]
null
null
null
null
Methyl 3-(4,7-difluoro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate was prepared (0.27 g, 31%) in the same manner as described in the above example 5. (1) from methyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (0.47 g, 2.47 mmol) and 3,6-difluorophthalic anhydride (0.50 g, 2.72 ...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Ester.Ester.Primary amine
Substituted dicarboximide
c1ccc2c(c1)COC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2.C1COCO1
HO-
null
null
null
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c(F)ccc(F)c21>>COC(=O)C(CN1C(=O)c2c(F)ccc(F)c2C1=O)C1(C)OCCO1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-12877900e40941db975f259d46996cee
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c1cccc2[N+](=O)[O-]>>COC(=O)C(CN1C(=O)c2cccc([N+](=O)[O-])c2C1=O)C1(C)OCCO1
NCC(C(=O)OC)C1(OCCO1)C.[N+](=O)([O-])C1=C2C(C(=O)OC2=O)=CC=C1>>[N+](=O)([O-])C1=C2C(N(C(C2=CC=C1)=O)CC(C(=O)OC)C1(OCCO1)C)=O
[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][NH2:7])[C:21]1([CH3:22])[O:23][CH2:24][CH2:25][O:26]1.O1[C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([N+:15](=[O:16])[O-:17])[c:18]2[C:19]1=[O:20]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][N:7]1[C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([N+:15](=[O:16])[O-:17])[c:18]2[C:19...
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c1cccc2[N+](=O)[O-]
COC(=O)C(CN1C(=O)c2cccc([N+](=O)[O-])c2C1=O)C1(C)OCCO1
null
null
null
Acylation
Phthalic anhydride to phthalimide
c3c986d6e09320348d40a4a59ca107882ce771f249842049dc55e55f334c675b
2bbbf7b24648445e31d33a2a26f8618c2067bd23957587cc459f3c45a03ed48a
O=C1c2ccccc2C(=O)N1CCC1OCCO1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[NH2;D1;+0:6].[O;D1;H0:7]=[C;H0;D3;+0:8]1-O-[C;H0;D3;+0:9](=[O;D1;H0:10])-[c:11](:[c:12]):[c:13]-1:[c:14]>>[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[N;H0;D3;+0:6]1-[C;H0;D3;+0:8](=[O;D1;H0:7])-[c:13](:[c:14]):[c:11](:[c:12])-[C;H0;D3;+0:9]-1=[O;D1;H0:10]
null
[]
null
null
null
null
Methyl 3-(4-nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate was prepared (0.27 g, 28%) in the same manner as described in the above example 5 (1) from methyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (0.50 g, 2.64 mmol) and 3-nitrophthalic anhydride (0.57 g, 3.43 mmol), and ...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Ester.Ester.Primary amine
Substituted dicarboximide
c1ccc2c(c1)COC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2.C1COCO1
HO-
null
null
null
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2c1cccc2[N+](=O)[O-]>>COC(=O)C(CN1C(=O)c2cccc([N+](=O)[O-])c2C1=O)C1(C)OCCO1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7191e37235674d979dcb6209ad9e8a6c
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2cc([N+](=O)[O-])ccc21>>COC(=O)C(CN1C(=O)c2ccc([N+](=O)[O-])cc2C1=O)C1(C)OCCO1
NCC(C(=O)OC)C1(OCCO1)C.[N+](=O)([O-])C=1C=C2C(C(=O)OC2=O)=CC1>>[N+](=O)([O-])C=1C=C2C(N(C(C2=CC1)=O)CC(C(=O)OC)C1(OCCO1)C)=O
[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][NH2:7])[C:21]1([CH3:22])[O:23][CH2:24][CH2:25][O:26]1.O1[C:8](=[O:9])[c:10]2[cH:11][cH:12][c:13]([N+:14](=[O:15])[O-:16])[cH:17][c:18]2[C:19]1=[O:20]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][N:7]1[C:8](=[O:9])[c:10]2[cH:11][cH:12][c:13]([N+:14](=[O:15])[O-:16])[cH:17][c:18]2[C:19...
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2cc([N+](=O)[O-])ccc21
COC(=O)C(CN1C(=O)c2ccc([N+](=O)[O-])cc2C1=O)C1(C)OCCO1
null
null
null
Acylation
Phthalic anhydride to phthalimide
c3c986d6e09320348d40a4a59ca107882ce771f249842049dc55e55f334c675b
2bbbf7b24648445e31d33a2a26f8618c2067bd23957587cc459f3c45a03ed48a
O=C1c2ccccc2C(=O)N1CCC1OCCO1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[NH2;D1;+0:6].[O;D1;H0:7]=[C;H0;D3;+0:8]1-O-[C;H0;D3;+0:9](=[O;D1;H0:10])-[c:11](:[c:12]):[c:13]-1:[c:14]>>[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[N;H0;D3;+0:6]1-[C;H0;D3;+0:8](=[O;D1;H0:7])-[c:13](:[c:14]):[c:11](:[c:12])-[C;H0;D3;+0:9]-1=[O;D1;H0:10]
null
[]
null
null
null
null
Methyl 3-(5-nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate was prepared (1.60 g, 42%) in the same manner as described in the above example 5 (1) from methyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (2.00 g, 10.57 mmol) and 4-nitrophthalic anhydride (0.57 g, 3.43 mmol), and...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Ester.Ester.Primary amine
Substituted dicarboximide
c1ccc2c(c1)COC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2.C1COCO1
HO-
null
null
null
COC(=O)C(CN)C1(C)OCCO1.O=C1OC(=O)c2cc([N+](=O)[O-])ccc21>>COC(=O)C(CN1C(=O)c2ccc([N+](=O)[O-])cc2C1=O)C1(C)OCCO1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3fcb315f756a4cc1aaa896443067c62d
COC(=O)C(CN)C1(C)OCCO1.Cc1cccc2c1C(=O)OC2=O>>COC(=O)C(CN1C(=O)c2cccc(C)c2C1=O)C1(C)OCCO1
NCC(C(=O)OC)C1(OCCO1)C.CC1=C2C(C(=O)OC2=O)=CC=C1>>CC1=C2C(N(C(C2=CC=C1)=O)CC(C(=O)OC)C1(OCCO1)C)=O
[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][NH2:7])[C:19]1([CH3:20])[O:21][CH2:22][CH2:23][O:24]1.O1[C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([CH3:15])[c:16]2[C:17]1=[O:18]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][N:7]1[C:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([CH3:15])[c:16]2[C:17]1=[O:18])[C:19]1([CH3:20])[O:...
COC(=O)C(CN)C1(C)OCCO1.Cc1cccc2c1C(=O)OC2=O
COC(=O)C(CN1C(=O)c2cccc(C)c2C1=O)C1(C)OCCO1
null
null
null
Acylation
Phthalic anhydride to phthalimide
c3c986d6e09320348d40a4a59ca107882ce771f249842049dc55e55f334c675b
2bbbf7b24648445e31d33a2a26f8618c2067bd23957587cc459f3c45a03ed48a
O=C1c2ccccc2C(=O)N1CCC1OCCO1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[NH2;D1;+0:6].[O;D1;H0:7]=[C;H0;D3;+0:8]1-O-[C;H0;D3;+0:9](=[O;D1;H0:10])-[c:11](:[c:12]):[c:13]-1:[c:14]>>[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[N;H0;D3;+0:6]1-[C;H0;D3;+0:8](=[O;D1;H0:7])-[c:13](:[c:14]):[c:11](:[c:12])-[C;H0;D3;+0:9]-1=[O;D1;H0:10]
null
[]
null
null
null
null
Methyl 3-(4-methyl-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate was prepared (0.39 g, 52%) in the same manner as described in the above example 5 (1) from methyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (0.54 g, 2.86 mmol) and 3-methylphthalic anhydride (0.56 g, 3.44 mmol), an...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Ester.Ester.Primary amine
Substituted dicarboximide
c1ccc2c(c1)COC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2.C1COCO1
HO-
null
null
null
COC(=O)C(CN)C1(C)OCCO1.Cc1cccc2c1C(=O)OC2=O>>COC(=O)C(CN1C(=O)c2cccc(C)c2C1=O)C1(C)OCCO1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-df42ecd09d73439fb486c4a6729824bb
COC(=O)C(CN)C1(C)OCCO1.Cc1ccc2c(c1)C(=O)OC2=O>>COC(=O)C(CN1C(=O)c2ccc(C)cc2C1=O)C1(C)OCCO1
NCC(C(=O)OC)C1(OCCO1)C.CC=1C=C2C(C(=O)OC2=O)=CC1>>CC=1C=C2C(N(C(C2=CC1)=O)CC(C(=O)OC)C1(OCCO1)C)=O
[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][NH2:7])[C:19]1([CH3:20])[O:21][CH2:22][CH2:23][O:24]1.O1[C:8](=[O:9])[c:10]2[cH:11][cH:12][c:13]([CH3:14])[cH:15][c:16]2[C:17]1=[O:18]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][N:7]1[C:8](=[O:9])[c:10]2[cH:11][cH:12][c:13]([CH3:14])[cH:15][c:16]2[C:17]1=[O:18])[C:19]1([CH3:20])[O:...
COC(=O)C(CN)C1(C)OCCO1.Cc1ccc2c(c1)C(=O)OC2=O
COC(=O)C(CN1C(=O)c2ccc(C)cc2C1=O)C1(C)OCCO1
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null
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Acylation
Phthalic anhydride to phthalimide
c3c986d6e09320348d40a4a59ca107882ce771f249842049dc55e55f334c675b
2bbbf7b24648445e31d33a2a26f8618c2067bd23957587cc459f3c45a03ed48a
O=C1c2ccccc2C(=O)N1CCC1OCCO1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[NH2;D1;+0:6].[O;D1;H0:7]=[C;H0;D3;+0:8]1-O-[C;H0;D3;+0:9](=[O;D1;H0:10])-[c:11](:[c:12]):[c:13]-1:[c:14]>>[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[N;H0;D3;+0:6]1-[C;H0;D3;+0:8](=[O;D1;H0:7])-[c:13](:[c:14]):[c:11](:[c:12])-[C;H0;D3;+0:9]-1=[O;D1;H0:10]
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Methyl 3-(5-methyl-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate was prepared (0.12 g, 10%) in the same manner as described in the above example 5 (1) from methyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (0.50 g, 2.64 mmol) and 4-methylphthalic anhydride (0.56 g, 3.43 mmol), an...
10.6084/m9.figshare.5104873.v1
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Anhydride.Ester.Ester.Primary amine
Substituted dicarboximide
c1ccc2c(c1)COC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2.C1COCO1
HO-
null
null
null
COC(=O)C(CN)C1(C)OCCO1.Cc1ccc2c(c1)C(=O)OC2=O>>COC(=O)C(CN1C(=O)c2ccc(C)cc2C1=O)C1(C)OCCO1