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-eb92e10054a6426ebcb60995047ce53d
Cc1cc(SCC=C(c2ccc(Br)cc2)c2ccc(Br)cc2)ccc1OCC(=O)O.OB(O)c1ccc(-c2ccccc2)cc1>>Cc1cc(SCC=C(c2ccc(-c3ccc(-c4ccccc4)cc3)cc2)c2ccc(-c3ccc(-c4ccccc4)cc3)cc2)ccc1OCC(=O)O
BrC1=CC=C(C=C1)C(=CCSC1=CC(=C(OCC(=O)O)C=C1)C)C1=CC=C(C=C1)Br.B(C=1C=CC(=CC1)C=2C=CC=CC2)(O)O.[F-].[K+].[Cl-].[NH4+]>>C1(=CC=C(C=C1)C(=CCSC1=CC(=C(OCC(=O)O)C=C1)C)C1=CC=C(C=C1)C1=CC=C(C=C1)C1=CC=CC=C1)C1=CC=C(C=C1)C1=CC=CC=C1
Br[c:12]1[cH:11][cH:10][c:9]([C:8](=[CH:7][CH2:6][S:5][c:4]2[cH:3][c:2]([CH3:1])[c:47]([O:48][CH2:49][C:50](=[O:51])[OH:52])[cH:46][cH:45]2)[c:27]2[cH:13][cH:29][c:30](Br)[cH:43][cH:44]2)[cH:26][cH:25]1.OB(O)[c:34]1[cH:14][cH:15][c:16](-[c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[cH:23][cH:41]1>>[CH3:1][c:2]1[cH:3][c:...
Cc1cc(SCC=C(c2ccc(Br)cc2)c2ccc(Br)cc2)ccc1OCC(=O)O.OB(O)c1ccc(-c2ccccc2)cc1
Cc1cc(SCC=C(c2ccc(-c3ccc(-c4ccccc4)cc3)cc2)c2ccc(-c3ccc(-c4ccccc4)cc3)cc2)ccc1OCC(=O)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].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
C1CCOC1
C-C Coupling
OtherReaction
a52ac3e68168ca2e107f5652b3de2c779a4e5fb59258bdf298eab75ddc044749
b431b00445693c7ae33759145152dfe407ee85c3562148bfc9cb7e8a06213bb6
C(CSc1ccccc1)=C(c1ccc(-c2ccc(-c3ccccc3)cc2)cc1)c1ccc(-c2ccc(-c3ccccc3)cc2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](-[C:5](=[C:6]-[C:7])-[c;H0;D3;+0:8]2:[c:9]:[c:10]:[c;H0;D3;+0:11](-Br):[cH;D2;+0:12]:[cH;D2;+0:13]:2):[c:14]:[c:15]:1.O-B(-O)-[c;H0;D3;+0:16]1:[cH;D2;+0:17]:[c:18]:[c:19](-[c:20]):[cH;D2;+0:21]:[cH;D2;+0:22]:1>>[C:7]-[C:6]=[C:5](-[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]2:[...
null
[]
50
CELSIUS
2
HOUR
In an evaporated schlenk flask kept under nitrogen atmosphere were added {4-[3,3-bis-(4-bromo-phenyl)-allylsulfanyl]-2-methyl-phenoxy}-acetic acid (225 mg, 0.41 mmol, example 1, step A–B, biphenylboronic acid (163 mg, 0.8 mmol), KF (79 mg, 1.35 mmol), Pd2(dba)3 (23 mg, 25 mmol) and Pd(P(t-Bu)3)2 (26 mg, 51 mmol). THF (...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Boronic acid
null
c1ccccc1.c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
Br-.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].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.C1CCOC1
50
2
Cc1cc(SCC=C(c2ccc(Br)cc2)c2ccc(Br)cc2)ccc1OCC(=O)O.OB(O)c1ccc(-c2ccccc2)cc1>C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].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.C1CCOC1>Cc1cc(SCC=C(c2ccc(-c3ccc(-c4ccccc4)cc3)...
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c5ebe0b0aed846cc89d4466e7663f9a1
CCOC(=O)COc1ccc(S)cc1C(F)(F)F.OCC=C(c1ccc(-c2cccnc2)cc1)c1ccc(-c2cccnc2)cc1>>CCOC(=O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F
C(C)OC(COC1=C(C=C(C=C1)S)C(F)(F)F)=O.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1CCN(CC1)C(=O)N=NC(=O)N2CCCCC2.N1=CC(=CC=C1)C1=CC=C(C=C1)C(=CCO)C1=CC=C(C=C1)C=1C=NC=CC1>>C(C)OC(COC1=C(C=C(C=C1)SCC=C(C1=CC=C(C=C1)C=1C=NC=CC1)C1=CC=C(C=C1)C=1C=NC=CC1)C(F)(F)F)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][O:7][c:8]1[cH:9][cH:10][c:11]([SH:12])[cH:40][c:41]1[C:42]([F:43])([F:44])[F:45].O[CH2:13][CH:14]=[C:15]([c:16]1[cH:17][cH:18][c:19](-[c:20]2[cH:21][cH:22][cH:23][n:24][cH:25]2)[cH:26][cH:27]1)[c:28]1[cH:29][cH:30][c:31](-[c:32]2[cH:33][cH:34][cH:35][n:36][cH:37]2)[cH:38][cH:39]1...
CCOC(=O)COc1ccc(S)cc1C(F)(F)F.OCC=C(c1ccc(-c2cccnc2)cc1)c1ccc(-c2cccnc2)cc1
CCOC(=O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
c119424abb7b621e5fb126e8156c5e4310815e8f2d609f48f2eb427b327d29ac
c1ccf05c97341d9cf75acae4c03f7d5a8212340a35905af6c8d60b4ccc775d1f
C(CSc1ccccc1)=C(c1ccc(-c2cccnc2)cc1)c1ccc(-c2cccnc2)cc1
O-[CH2;D2;+0:1]-[C:2]=[C:3](-[c:4])-[c:5].[SH;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[c:8]:[c:7](-[S;H0;D2;+0:6]-[CH2;D2;+0:1]-[C:2]=[C:3](-[c:4])-[c:5]):[c:9]
null
[]
null
null
5
MINUTE
Triphenylphosphine (138 mg, 0.68 mmol) and ADDP (173 mg, 0.68 mmol) were added to a solution of 3,3-bis-(4-pyridin-3-yl-phenyl)-prop-2-en-1-ol (100 mg, 0.27 mmol) in THF (5 ml) at 0° C. The reaction mixture was stirred for 5 min under nitrogen atmosphere. (4-Mercapto-2-trifluoromethyl-phenoxy)-acetic acid ethyl ester (...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic thiol
Monosulfide
null
null
c1ccccc1.c1ccccc1.c1ccncc1.c1ccccc1.c1ccncc1
HO-
C1CCOC1
null
0.083333
CCOC(=O)COc1ccc(S)cc1C(F)(F)F.OCC=C(c1ccc(-c2cccnc2)cc1)c1ccc(-c2cccnc2)cc1>C1CCOC1>CCOC(=O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e72a29a49a7e4e14b6c97a72e07036ea
CCOC(=O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F>>O=C(O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F
C(C)OC(COC1=C(C=C(C=C1)SCC=C(C1=CC=C(C=C1)C=1C=NC=CC1)C1=CC=C(C=C1)C=1C=NC=CC1)C(F)(F)F)=O>>N1=CC(=CC=C1)C1=CC=C(C=C1)C(=CCSC1=CC(=C(OCC(=O)O)C=C1)C(F)(F)F)C1=CC=C(C=C1)C=1C=NC=CC1
CC[O:3][C:2](=[O:1])[CH2:4][O:5][c:6]1[cH:7][cH:8][c:9]([S:10][CH2:11][CH:12]=[C:13]([c:14]2[cH:15][cH:16][c:17](-[c:18]3[cH:19][cH:20][cH:21][n:22][cH:23]3)[cH:24][cH:25]2)[c:26]2[cH:27][cH:28][c:29](-[c:30]3[cH:31][cH:32][cH:33][n:34][cH:35]3)[cH:36][cH:37]2)[cH:38][c:39]1[C:40]([F:41])([F:42])[F:43]>>[O:1]=[C:2]([OH...
CCOC(=O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F
O=C(O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F
null
null
[OH-].[Na+].C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
C(CSc1ccccc1)=C(c1ccc(-c2cccnc2)cc1)c1ccc(-c2cccnc2)cc1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
A solution of {4-[3,3-bis-(4-pyridin-3-yl-phenyl)-allylsulfanyl]-2-trifluoromethyl-phenoxy}-acetic acid ethyl ester (70 mg, 0.1 mmol) in ethanol (10 ml) and 1N NaOH (0.5 ml) was stirred at 75° C. for 1 h. The reaction mixture was evaporated and the residue was treated with 1N HCl (0.7 ml) and extracted with methylene c...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccccc1.c1ccncc1.c1ccccc1.c1ccncc1
Other
[OH-].[Na+].C(C)O
null
null
CCOC(=O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F>[OH-].[Na+].C(C)O>O=C(O)COc1ccc(SCC=C(c2ccc(-c3cccnc3)cc2)c2ccc(-c3cccnc3)cc2)cc1C(F)(F)F
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-25de6e20d68e4a01a05d61c43866a6f5
CC1(C)OC(=O)CC(=O)O1.Nc1cccc(Br)c1>>CC1(C)OC(=O)C(=CNc2cccc(Br)c2)C(=O)O1
C(OCC)(OCC)OCC.CC1(OC(=O)CC(=O)O1)C.BrC=1C=C(N)C=CC1.BrC=1C=C(N)C=CC1>>BrC=1C=C(C=CC1)NC=C1C(OC(OC1=O)(C)C)=O
[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[CH2:7][C:17](=[O:18])[O:19]1.[NH2:9][c:10]1[cH:11][cH:12][cH:13][c:14]([Br:15])[cH:16]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[C:7](=[CH:8][NH:9][c:10]2[cH:11][cH:12][cH:13][c:14]([Br:15])[cH:16]2)[C:17](=[O:18])[O:19]1
CC1(C)OC(=O)CC(=O)O1.Nc1cccc(Br)c1
CC1(C)OC(=O)C(=CNc2cccc(Br)c2)C(=O)O1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
16f6e689ff4988a3075463cf8c372a4929ef73d83eb11dd6443a2ba775713df7
cb45d3f2664ea1c07edca6192a95c91d6c98f4c61196cc5a896d41447e7a94b5
O=C1OCOC(=O)C1=CNc1ccccc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C:6]1-[#8:7]-[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[CH2;D2;+0:12]-1>>[O;D1;H0:5]=[C:6]1-[#8:7]-[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[C;H0;D3;+0:12]-1=[C:13]-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
55
CELSIUS
null
null
A mixture of triethyl orthoformate (154 grams (g), 1.04 moles (mol) and Meldrum's acid (142 g, 0.983 mol) was heated to 55° C. for 4 hours (h). After cooling to 50° C., a solution of 3-bromoaniline (162.6 g, 0.945 mol) in ethanol (300 mL) was added such that the temperature of the reaction was maintained between 50–55°...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Primary amine
Enamine
C1COCOC1
C1COCOC1
C1COCOC1.c1ccccc1
Other
C(C)O
55
null
CC1(C)OC(=O)CC(=O)O1.Nc1cccc(Br)c1>C(C)O>CC1(C)OC(=O)C(=CNc2cccc(Br)c2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b3f9f78625db481c835ecd681b30b45a
O=[N+]([O-])O.Oc1ccnc2cc(Br)ccc12>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1O
BrC1=CC=C2C(=CC=NC2=C1)O.[N+](=O)(O)[O-].[N+](=O)(O)[O-]>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])O
O[N+:2](=[O:1])[O-:3].[cH:4]1[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]2[c:14]1[OH:15]>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]2[c:14]1[OH:15]
O=[N+]([O-])O.Oc1ccnc2cc(Br)ccc12
O=[N+]([O-])c1cnc2cc(Br)ccc2c1O
null
null
C(CC)(=O)O
Functional Group Addition
Aromatic nitration with HNO3
93c60f395fb4f0e5be7b3c9f5aae0bbd322ad57344c0d8df26b336a54b906179
ddce49825c02b8965f10c8d99e3c841d26e1f136da6037b417c09313e6d73097
c1ccc2ncccc2c1
O-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3].[O;D1;H1:4]-[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[cH;D2;+0:10]:1>>[O;-;D1;H0:2]-[N+;H0;D3:1](=[O;D1;H0:3])-[c;H0;D3;+0:10]1:[c:9]:[#7;a:8]:[c:7]:[c:6]:[c:5]:1-[O;D1;H1:4]
78.1
[{"value": 78.1, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A stirred suspension of 7-bromoquinolin-4-ol (162 g, 0.723 mol) in propionic acid (1500 mL) was brought to 110° C. 70% Nitric acid (85 g) was added dropwise over 1 h such that the temperature was maintained between 110–115° C. After half of the nitric acid had been added, stirring became difficult due to the formation ...
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HO-
C(CC)(=O)O
null
null
O=[N+]([O-])O.Oc1ccnc2cc(Br)ccc12>C(CC)(=O)O>O=[N+]([O-])c1cnc2cc(Br)ccc2c1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-124d1086d4d44e1a9c954932a0b1a5e1
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1O>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])O.O=P(Cl)(Cl)Cl>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl
O=P(Cl)(Cl)[Cl:15].O[c:14]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]2[c:14]1[Cl:15]
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1O
O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
null
null
null
Functional Group Interconversion
Alcohol to chloride_POCl3_para
27014e1419adc48e7dd5f2024d7f933bb85e42d4ec6c57e509da2884d477d689
e71580a8ffadb7b2717ecd7d68c1d3c0ca161ba5e6a787a49dad5a1359adc993
c1ccc2ncccc2c1
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].O-[c;H0;D3;+0:2]1:[c:3](:[c:4]):[c:5](:[c:6]):[#7;a:7]:[c:8]:[c:9]:1-[#7;+:10]>>[#7;+:10]-[c:9]1:[c:8]:[#7;a:7]:[c:5](:[c:6]):[c:3](:[c:4]):[c;H0;D3;+0:2]:1-[Cl;H0;D1;+0:1]
null
[]
null
null
45
MINUTE
7-Bromo-3-nitroquinolin-4-ol (42 g, 156 millimoles (mmol)) was suspended in POCl3 (130 mL) and brought to 102° C. under an atmosphere of N2. After 45 min, all of the solids had dissolved, so the reaction was cooled to room temperature (RT). The resulting solids were collected by filtration, washed with H2O, and then pa...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol
Aromatic halide
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
null
null
0.75
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1O>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-630f53709a7641e4abb79b3ac6370174
CC(C)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>CC(C)CNc1c(N)cnc2cc(Br)ccc12
[O-]S(=O)S(=O)[O-].[Na+].[Na+].BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC(C)C>>BrC1=CC=C2C(=C(C=NC2=C1)N)NCC(C)C
O=[N+:8]([O-])[c:7]1[c:6]([NH:5][CH2:4][CH:2]([CH3:1])[CH3:3])[c:17]2[c:11]([n:10][cH:9]1)[cH:12][c:13]([Br:14])[cH:15][cH:16]2>>[CH3:1][CH:2]([CH3:3])[CH2:4][NH:5][c:6]1[c:7]([NH2:8])[cH:9][n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]12
CC(C)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
CC(C)CNc1c(N)cnc2cc(Br)ccc12
null
null
O.C(C)(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2ncccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
135.6
[{"value": 135.6, "product": "BrC1=CC=C2C(=C(C=NC2=C1)N)NCC(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of Na2S2O4 (193 g) in H2O (1 L) was added to a boiling solution of (7-bromo-3-nitroquinolin-4-yl)isobutylamine (32.0 g, 99 mmol) in isopropanol (1 L). Upon complete addition, the reaction mixture was cooled to room temperature and the bulk of the isopropanol was removed on a rotary evaporator. The resulting ...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
O.C(C)(C)O
null
null
CC(C)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>O.C(C)(C)O>CC(C)CNc1c(N)cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-162be3fc5e3f4ed98a5683cec7677ead
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCCCC(OC)(OC)OC>>CCCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
BrC1=CC=C2C(=C(C=NC2=C1)N)NCC(C)C.C(CCCC)(OC)(OC)OC>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)C)CCCC
[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]2[c:17]1[NH:18][CH2:19][CH:20]([CH3:21])[CH3:22].CO[C:5](OC)(OC)[CH2:4][CH2:3][CH2:2][CH3:1]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH:20]([CH3:21])[CH3:22]
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCCCC(OC)(OC)OC
CCCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
null
Cl.N1=CC=CC=C1
C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
8d87c769e65778c9400c7f523e0409ecf0ffad86543cd9fdd6ef4b239323db96
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc2c(c1)ncc1nc[nH]c12
C-O-[C;H0;D4;+0:1](-O-C)(-O-C)-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
43.9
[{"value": 43.9, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)C)CCCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7-Bromo-N4-isobutylquinoline-3,4-diamine (39.4 g of crude material), trimethyl orthovalerate (32 g, 0.20 mol), and pyridine hydrochloride (0.31 g, 2.7 mmol) were combined with anhydrous toluene (500 mL) and heated to reflux for 30 min. The reaction was cooled to room temperature, concentrated, and the residue was purif...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
HO-
Cl.N1=CC=CC=C1.C1(=CC=CC=C1)C
null
null
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCCCC(OC)(OC)OC>Cl.N1=CC=CC=C1.C1(=CC=CC=C1)C>CCCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fbc47495747e4abfa9aa3c4624c34f3b
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)c1ccccc1>>CCCCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC(C)C
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCCC.C1(=CC=CC=C1)B(O)O>>C(CCC)C=1N(C2=C(C(=NC=3C=C(C=CC23)C2=CC=CC=C2)N)N1)CC(C)C
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][CH2:3][CH2:2][CH3:1])[n:24]([CH2:25][CH:26]([CH3:27])[CH3:28])[c:23]3[c:22]2[cH:21][cH:20]1.OB(O)[c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][c...
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)c1ccccc1
CCCCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC(C)C
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
89ee2e97ba79660eddf3dfa788334e60a83082a3d4afa6ed050c5f1f85789150
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3c(c2)ncc2nc[nH]c23)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)-[c;H0;D3;+0:13](:[c:14]:[c:15]):[c:16]:[c:17]>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13](:[c:14]:[c:15]):[c:16]:[c:17]):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1:[#7;a:7]
null
[]
null
null
null
null
7-Bromo-2-butyl-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and benzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. Purification by chromatography on silica gel (20% acetone in toluene to 60% acetone in toluene gradient) afforded 2-butyl-1-isobutyl-7-phenyl-1H-imidazo[...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HBr.B
null
null
null
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)c1ccccc1>>CCCCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0657f11f0a2c4022942778090163fb5a
CCCCc1nc2cnc3cc(-c4ccc(OC)cc4OC)ccc3c2n1CC(C)C.CCCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C.COc1ccc(B(O)O)c(OC)c1>>CCCCc1nc2c(N)nc3cc(-c4ccc(OC)cc4OC)ccc3c2n1CC(C)C
BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)C)CCCC.COC1=C(C=CC(=C1)OC)B(O)O.C(CCC)C=1N(C2=C(C=NC=3C=C(C=CC23)C2=C(C=C(C=C2)OC)OC)N1)CC(C)C>>C(CCC)C=1N(C2=C(C(=NC=3C=C(C=CC23)C2=C(C=C(C=C2)OC)OC)N)N1)CC(C)C
COc1ccc(-[c:13]2[cH:12][c:11]3[n:9][cH:8][c:7]4[n:6][c:5]([CH2:4][CH2:3][CH2:2][CH3:1])[n:28]([CH2:29][CH:30]([CH3:31])[CH3:32])[c:27]4[c:26]3[cH:25][cH:24]2)c(OC)c1.CCCCc1nc2c[n:10]c3cc(Br)ccc3c2n1CC(C)C.OB(O)[c:14]1[cH:15][cH:16][c:17]([O:18][CH3:19])[cH:20][c:21]1[O:22][CH3:23]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:...
CCCCc1nc2cnc3cc(-c4ccc(OC)cc4OC)ccc3c2n1CC(C)C.CCCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C.COc1ccc(B(O)O)c(OC)c1
CCCCc1nc2c(N)nc3cc(-c4ccc(OC)cc4OC)ccc3c2n1CC(C)C
null
null
null
C-C Coupling
OtherReaction
cb4cc0022a7341fde0f95bc21a175e59667459f7912fea6931da43876194ab9c
211bc1f53e80deec1d6ffae932269931f18571c43be73f2a28a363359aa16d14
c1ccc(-c2ccc3c(c2)ncc2nc[nH]c23)cc1
Br-c1:c:c:c2:c(:[n;H0;D2;+0:1]:c:c3:n:c(-C-C-C-C):n(-C-C(-C)-C):c:3:2):c:1.C-O-c1:c:c:c(-[c;H0;D3;+0:2]2:[c:3]:[c;H0;D3;+0:4]3:[n;H0;D2;+0:5]:[cH;D2;+0:6]:[c:7]4:[#7;a:8]:[c:9]:[#7;a:10](-[C:11]):[c:12]:4:[c:13]:3:[c:14]:[c:15]:2):c(-O-C):c:1.O-B(-O)-[c;H0;D3;+0:16](:[c:17]:[c:18]):[c:19](-[#8:20]):[c:21]>>[#8:20]-[c:1...
null
[]
null
null
null
null
7-Bromo-2-butyl-1-isobutyl-1H-imidazo[4,5-c]quinoline and 2,4-dimethoxybenzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. The resulting 2-butyl-7-(2,4-dimethoxyphenyl)-1-isobutyl-1H-imidazo[4,5-c]quinoline was oxidized and then aminated according to the general procedu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ether.Ether.Boronic acid
Primary amine
c1ccccc1.c1ccc2c(c1)ncc1[nH]cnc12.c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HBr.B
null
null
null
CCCCc1nc2cnc3cc(-c4ccc(OC)cc4OC)ccc3c2n1CC(C)C.CCCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C.COc1ccc(B(O)O)c(OC)c1>>CCCCc1nc2c(N)nc3cc(-c4ccc(OC)cc4OC)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-182ec36ce0ca4c7dba7b593a28732964
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.CCCOc1ccc(B(O)O)cc1>>CCCCc1nc2c(N)nc3cc(-c4ccc(OCCC)cc4)ccc3c2n1CC(C)C
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCCC.C(CC)OC1=CC=C(C=C1)B(O)O>>C(CCC)C=1N(C2=C(C(=NC=3C=C(C=CC23)C2=CC=C(C=C2)OCCC)N)N1)CC(C)C
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][CH2:3][CH2:2][CH3:1])[n:28]([CH2:29][CH:30]([CH3:31])[CH3:32])[c:27]3[c:26]2[cH:25][cH:24]1.OB(O)[c:14]1[cH:15][cH:16][c:17]([O:18][CH2:19][CH2:20][CH3:21])[cH:22][cH:23]1>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12]...
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.CCCOc1ccc(B(O)O)cc1
CCCCc1nc2c(N)nc3cc(-c4ccc(OCCC)cc4)ccc3c2n1CC(C)C
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
89ee2e97ba79660eddf3dfa788334e60a83082a3d4afa6ed050c5f1f85789150
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3c(c2)ncc2nc[nH]c23)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)-[c;H0;D3;+0:13](:[c:14]:[c:15]):[c:16]:[c:17]>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13](:[c:14]:[c:15]):[c:16]:[c:17]):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1:[#7;a:7]
null
[]
null
null
null
null
7-Bromo-2-butyl-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and 4-propoxybenzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. The product was recrystallized from isopropanol, collected by filtration, dissolved in CH2Cl2, and then precipitated with hexanes to afford 2-bu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HBr.B
null
null
null
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.CCCOc1ccc(B(O)O)cc1>>CCCCc1nc2c(N)nc3cc(-c4ccc(OCCC)cc4)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c102d39a905743a7a2a47a58a5ea662c
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.CCCOc1ccccc1B(O)O>>CCCCc1nc2c(N)nc3cc(-c4ccccc4OCCC)ccc3c2n1CC(C)C
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCCC.C(CC)OC1=C(C=CC=C1)B(O)O>>C(CCC)C=1N(C2=C(C(=NC=3C=C(C=CC23)C2=C(C=CC=C2)OCCC)N)N1)CC(C)C
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][CH2:3][CH2:2][CH3:1])[n:28]([CH2:29][CH:30]([CH3:31])[CH3:32])[c:27]3[c:26]2[cH:25][cH:24]1.OB(O)[c:14]1[cH:15][cH:16][cH:17][cH:18][c:19]1[O:20][CH2:21][CH2:22][CH3:23]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c...
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.CCCOc1ccccc1B(O)O
CCCCc1nc2c(N)nc3cc(-c4ccccc4OCCC)ccc3c2n1CC(C)C
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
89ee2e97ba79660eddf3dfa788334e60a83082a3d4afa6ed050c5f1f85789150
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3c(c2)ncc2nc[nH]c23)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)-[c;H0;D3;+0:13](:[c:14]:[c:15]):[c:16](-[#8:17]):[c:18]>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13](:[c:14]:[c:15]):[c:16](-[#8:17]):[c:18]):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1:[...
null
[]
null
null
null
null
7-Bromo-2-butyl-1-isobutyl-1 H-imidazo[4,5-c]quinolin-4-amine and 2-propoxybenzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. The product was recrystallized from isopropanol, collected by filtration, dissolved in CH2Cl2, and then precipitated with hexanes to afford 2-b...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HBr.B
null
null
null
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.CCCOc1ccccc1B(O)O>>CCCCc1nc2c(N)nc3cc(-c4ccccc4OCCC)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-df44df3856b445519b7fa8f4529264dd
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)/C=C/c1ccccc1>>CCCCc1nc2c(N)nc3cc(/C=C/c4ccccc4)ccc3c2n1CC(C)C
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCCC.C1(=CC=CC=C1)/C=C/B(O)O>>C(CCC)C=1N(C2=C(C(=NC=3C=C(C=CC23)\C=C\C2=CC=CC=C2)N)N1)CC(C)C
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][CH2:3][CH2:2][CH3:1])[n:26]([CH2:27][CH:28]([CH3:29])[CH3:30])[c:25]3[c:24]2[cH:23][cH:22]1.OB(O)/[CH:14]=[CH:15]/[c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](/[CH:14...
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)/C=C/c1ccccc1
CCCCc1nc2c(N)nc3cc(/C=C/c4ccccc4)ccc3c2n1CC(C)C
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
31390bd58c61a8b3a63a0fcb56e173272a33417778faf6071248245ca26329ae
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
C(=C/c1ccc2c(c1)ncc1nc[nH]c12)\c1ccccc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)/[CH;D2;+0:13]=[C:14]/[c:15](:[c:16]):[c:17]>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](/[CH;D2;+0:13]=[C:14]/[c:15](:[c:16]):[c:17]):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1:[#7;a:7]
null
[]
null
null
null
null
7-Bromo-2-butyl-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and trans-2-phenylvinylboronic acid were coupled according to the general procedure described in Part J of Example 1. Recrystallization from toluene followed by chromatography on silica gel (8% methanol in CH2Cl2) afforded 2-butyl-1-isobutyl-7-[(E)-2-phenylet...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HBr.B
null
null
null
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)/C=C/c1ccccc1>>CCCCc1nc2c(N)nc3cc(/C=C/c4ccccc4)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a10c8fa6f2f44d2892a4bdf1b6af3582
CCCCc1nc2c(N)nc3cc(/C=C/c4ccccc4)ccc3c2n1CC(C)C>>CCCCc1nc2c(N)nc3cc(CCc4ccccc4)ccc3c2n1CC(C)C
C(CCC)C=1N(C2=C(C(=NC=3C=C(C=CC23)\C=C\C2=CC=CC=C2)N)N1)CC(C)C>>C(CCC)C=1N(C2=C(C(=NC=3C=C(C=CC23)CCC2=CC=CC=C2)N)N1)CC(C)C
[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](/[CH:14]=[CH:15]/[c:16]4[cH:17][cH:18][cH:19][cH:20][cH:21]4)[cH:22][cH:23][c:24]3[c:25]2[n:26]1[CH2:27][CH:28]([CH3:29])[CH3:30]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13]([CH2:14][CH2:15][...
CCCCc1nc2c(N)nc3cc(/C=C/c4ccccc4)ccc3c2n1CC(C)C
CCCCc1nc2c(N)nc3cc(CCc4ccccc4)ccc3c2n1CC(C)C
null
[Pd]
null
Reduction
Hydrogenation (double to single)
0bc3968b35f0839c230afb4215314da278abd4e1f10e42ec3012c5512de49ea5
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1ccc(CCc2ccc3c(c2)ncc2nc[nH]c23)cc1
[#7;a:1]:[c:2]:[c:3]:[c:4](/[CH;D2;+0:5]=[CH;D2;+0:6]/[c:7](:[c:8]):[c:9]):[c:10]>>[#7;a:1]:[c:2]:[c:3]:[c:4](-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[c:7](:[c:8]):[c:9]):[c:10]
26.6
[{"value": 26.6, "product": "C(CCC)C=1N(C2=C(C(=NC=3C=C(C=CC23)CCC2=CC=CC=C2)N)N1)CC(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Butyl-1-isobutyl-7-[(E)-2-phenylethenyl]-1H-imidazo[4,5-c]quinolin-4-amine (562 mg, 1.41 mmol) was hydrogenated in a Parr bottle over palladium on carbon (10%) until the starting material was consumed as judged by high performance liquid chromatography (HPLC) and thin layer chromatography (TLC) analyses. Purification...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
null
[Pd]
null
null
CCCCc1nc2c(N)nc3cc(/C=C/c4ccccc4)ccc3c2n1CC(C)C>[Pd]>CCCCc1nc2c(N)nc3cc(CCc4ccccc4)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dbeb3e2c5d2e43e88e3b4fdfc8b56049
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
BrC1=CC=C2C(=C(C=NC2=C1)N)NCC(C)C.C(C)OCC(=O)Cl>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)C)COCC
[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]2[c:17]1[NH:18][CH2:19][CH:20]([CH3:21])[CH3:22].O=[C:5](Cl)[CH2:4][O:3][CH2:2][CH3:1]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH:20]([CH3:21])[CH3:22]
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
null
null
N1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
101a087a520f159c722ba3d78ed38f5c3c1cf154206e5edbeb1e6397c929560f
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[#8:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[#8:3]-[C:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:13]:[c:12]2:[c:11]:[#7;a:10]:[c:9]:[c:8]:[c:7]:2:[n;H0;D3;+0:6]:1-[C:5]-[C:4]
41.1
[{"value": 41.1, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)C)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3.5
HOUR
A solution of 7-bromo—N4-isobutylquinoline-3,4-diamine (85 g, prepared according to Part F of Example 1) in anhydrous pyridine (413 mL) was immersed in an ice bath, and ethoxyacetyl chloride (36.9 g, 300 mmol) was added. The reaction was allowed to warm to room temperature and was then heated in an oil bath held at 85°...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
HCl
N1=CC=CC=C1
null
3.5
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl>N1=CC=CC=C1>CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cf064ee4162445c1a8b080a1ce1d6cbd
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)c1ccsc1>>CCOCc1nc2c(N)nc3cc(-c4ccsc4)ccc3c2n1CC(C)C
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)COCC.S1C=C(C=C1)B(O)O>>C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C2=CSC=C2)N)N1)CC(C)C
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:23]([CH2:24][CH:25]([CH3:26])[CH3:27])[c:22]3[c:21]2[cH:20][cH:19]1.OB(O)[c:14]1[cH:15][cH:16][s:17][cH:18]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][s:17][cH:18]4...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)c1ccsc1
CCOCc1nc2c(N)nc3cc(-c4ccsc4)ccc3c2n1CC(C)C
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
71675559eb4d0d484707d6905401f948ae6ef7d05b7d29e48ea037255a256d18
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1nc2cnc3cc(-c4ccsc4)ccc3c2[nH]1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)-[c;H0;D3;+0:13]1:[c:14]:[c:15]:[#16;a:16]:[c:17]:1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]3:[c:14]:[c:15]:[#16;a:16]:[c:17]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1:[#7;a:7]
null
[]
null
null
null
null
7-Bromo-2-ethoxymethyl-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and thiophene-3-boronic acid were coupled according to the general procedure described in Part J of Example 1. Recrystallization from isopropanol followed by purification on silica gel (5% methanol in CH2Cl2 to 7% methanol in CH2Cl2 gradient) afforded ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccsc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccsc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccsc1
HBr.B
null
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.OB(O)c1ccsc1>>CCOCc1nc2c(N)nc3cc(-c4ccsc4)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-90677ea3c633433eb22e37de2541dc36
CC1(C)OC(=O)CC(=O)O1.Nc1cccc(-c2ccccc2)c1>>CC1(C)OC(=O)C(=CNc2cccc(-c3ccccc3)c2)C(=O)O1
C(OCC)(OCC)OCC.CC1(OC(=O)CC(=O)O1)C.C1(=CC(=CC=C1)N)C1=CC=CC=C1>>C1(=CC(=CC=C1)NC=C1C(OC(OC1=O)(C)C)=O)C1=CC=CC=C1
[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[CH2:7][C:22](=[O:23])[O:24]1.[NH2:9][c:10]1[cH:11][cH:12][cH:13][c:14](-[c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[cH:21]1>>[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[C:7](=[CH:8][NH:9][c:10]2[cH:11][cH:12][cH:13][c:14](-[c:15]3[cH:16][cH:17][cH:18][cH:19][cH:20]3)[cH:21]2)[C:22...
CC1(C)OC(=O)CC(=O)O1.Nc1cccc(-c2ccccc2)c1
CC1(C)OC(=O)C(=CNc2cccc(-c3ccccc3)c2)C(=O)O1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
16f6e689ff4988a3075463cf8c372a4929ef73d83eb11dd6443a2ba775713df7
cb45d3f2664ea1c07edca6192a95c91d6c98f4c61196cc5a896d41447e7a94b5
O=C1OCOC(=O)C1=CNc1cccc(-c2ccccc2)c1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4].[O;D1;H0:5]=[C:6]1-[#8:7]-[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[CH2;D2;+0:12]-1>>[O;D1;H0:5]=[C:6]1-[#8:7]-[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[C;H0;D3;+0:12]-1=[C:13]-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]
95.5
[{"value": 95.5, "product": "C1(=CC(=CC=C1)NC=C1C(OC(OC1=O)(C)C)=O)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Triethyl orthoformate (148 g, 1.00 mol), Meldrum's acid (137 g, 0.95 mol), and biphenyl-3-ylamine (155 g, 0.916 mol) were combined and treated according to the general procedure described in Part A of Example 1 to obtain 283 g of 5-(biphenyl-3-ylaminomethylene)-2,2-dimethyl-[1,3]dioxane-4,6-dione as a yellow solid. Con...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Primary amine
Enamine
C1COCOC1
C1COCOC1
C1COCOC1.c1ccccc1.c1ccccc1
Other
null
null
null
CC1(C)OC(=O)CC(=O)O1.Nc1cccc(-c2ccccc2)c1>>CC1(C)OC(=O)C(=CNc2cccc(-c3ccccc3)c2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0c1767eb462a4ef8a4aafe3f59af607c
CC1(C)OC(=O)C(=CNc2cccc(-c3ccccc3)c2)C(=O)O1>>Oc1ccnc2cc(-c3ccccc3)ccc12
C1(=CC(=CC=C1)NC=C1C(OC(OC1=O)(C)C)=O)C1=CC=CC=C1>>C1(=CC=CC=C1)C1=CC=C2C(=CC=NC2=C1)O
CC1(C)OC(=O)[C:3](=[CH:4][NH:5][c:6]2[cH:7][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)[cH:15][cH:16][cH:17]2)[C:2](=[O:1])O1>>[OH:1][c:2]1[cH:3][cH:4][n:5][c:6]2[cH:7][c:8](-[c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)[cH:15][cH:16][c:17]12
CC1(C)OC(=O)C(=CNc2cccc(-c3ccccc3)c2)C(=O)O1
Oc1ccnc2cc(-c3ccccc3)ccc12
null
null
C1=CC=C(C=C1)C2=CC=CC=C2.C1=CC=C(C=C1)OC2=CC=CC=C2
Reduction
OtherReaction
60da20daff3794d62e19d3191423fbc1080fe07b8a447f857ff8933cfafabe89
61086c5a1f033ee6da72542244d080a3c3d1d71db445f7bf1dc4b7c5fe1fe33e
c1ccc(-c2ccc3cccnc3c2)cc1
C-C1(-C)-O-C(=O)-[C;H0;D3;+0:1](=[CH;D2;+0:2]-[NH;D2;+0:3]-[c:4](:[c:5]):[cH;D2;+0:6]:[c:7]:[c:8])-[C;H0;D3;+0:9](=[O;H0;D1;+0:10])-O-1>>[OH;D1;+0:10]-[c;H0;D3;+0:9]1:[cH;D2;+0:1]:[cH;D2;+0:2]:[n;H0;D2;+0:3]:[c:4](:[c:5]):[c;H0;D3;+0:6]:1:[c:7]:[c:8]
96.7
[{"value": 96.7, "product": "C1(=CC=CC=C1)C1=CC=C2C(=CC=NC2=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
90
MINUTE
5-(Biphenyl-3-ylaminomethylene)-2,2-dimethyl-[1,3]dioxane-4,6-dione (160.2 g, 496 mmol) was dissolved in 800 mL of DOWTHERM A heat transfer fluid at 100° C. and added over 40 min by way of a cannula line to 1.3 L of preheated DOWTHERM A heat transfer fluid to 215° C. After complete addition, the reaction was held at 21...
10.6084/m9.figshare.5104873.v1
null
Enamine.Ester.Ester
Aromatic alcohol
C1COCOC1.c1ccccc1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HO-
C1=CC=C(C=C1)C2=CC=CC=C2.C1=CC=C(C=C1)OC2=CC=CC=C2
100
1.5
CC1(C)OC(=O)C(=CNc2cccc(-c3ccccc3)c2)C(=O)O1>C1=CC=C(C=C1)C2=CC=CC=C2.C1=CC=C(C=C1)OC2=CC=CC=C2>Oc1ccnc2cc(-c3ccccc3)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e52aec0cac81483fa1aff8a997e54a25
O=[N+]([O-])O.Oc1ccnc2cc(-c3ccccc3)ccc12>>O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1O
C1(=CC=CC=C1)C1=CC=C2C(=CC=NC2=C1)O.[N+](=O)(O)[O-]>>[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1O)C1=CC=CC=C1
O[N+:2](=[O:1])[O-:3].[cH:4]1[cH:5][n:6][c:7]2[cH:8][c:9](-[c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[cH:16][cH:17][c:18]2[c:19]1[OH:20]>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][c:9](-[c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[cH:16][cH:17][c:18]2[c:19]1[OH:20]
O=[N+]([O-])O.Oc1ccnc2cc(-c3ccccc3)ccc12
O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1O
null
null
C(CC)(=O)O
Functional Group Addition
Aromatic nitration with HNO3
93c60f395fb4f0e5be7b3c9f5aae0bbd322ad57344c0d8df26b336a54b906179
ddce49825c02b8965f10c8d99e3c841d26e1f136da6037b417c09313e6d73097
c1ccc(-c2ccc3cccnc3c2)cc1
O-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3].[O;D1;H1:4]-[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[cH;D2;+0:10]:1>>[O;-;D1;H0:2]-[N+;H0;D3:1](=[O;D1;H0:3])-[c;H0;D3;+0:10]1:[c:9]:[#7;a:8]:[c:7]:[c:6]:[c:5]:1-[O;D1;H1:4]
81.4
[{"value": 81.4, "product": "[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1O)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
129
CELSIUS
3
HOUR
A stirred suspension of 7-phenylquinolin-4-ol (84.9 g, 384 mmol) in propionic acid (850 mL) was heated to 129° C. Nitric acid (70%, 45.0 g) was added dropwise over 25 min, during which the temperature dropped to 124° C. The reaction was stirred an additional 3 h at that temperature and then cooled to 5° C. on an ice ba...
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HO-
C(CC)(=O)O
129
3
O=[N+]([O-])O.Oc1ccnc2cc(-c3ccccc3)ccc12>C(CC)(=O)O>O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ba70021346be4b7b8d28ff373488a299
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1O>>O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
P(=O)(Cl)(Cl)Cl.[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1O)C1=CC=CC=C1>>ClC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-]
O=P(Cl)(Cl)[Cl:20].O[c:19]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][c:9](-[c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[cH:16][cH:17][c:18]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][c:9](-[c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[cH:16][cH:17][c:18]2[c:19]1[Cl:20]
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1O
O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
null
null
CN(C=O)C
Functional Group Interconversion
Alcohol to chloride_POCl3_para
27014e1419adc48e7dd5f2024d7f933bb85e42d4ec6c57e509da2884d477d689
e71580a8ffadb7b2717ecd7d68c1d3c0ca161ba5e6a787a49dad5a1359adc993
c1ccc(-c2ccc3cccnc3c2)cc1
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].O-[c;H0;D3;+0:2]1:[c:3](:[c:4]):[c:5](:[c:6]):[#7;a:7]:[c:8]:[c:9]:1-[#7;+:10]>>[#7;+:10]-[c:9]1:[c:8]:[#7;a:7]:[c:5](:[c:6]):[c:3](:[c:4]):[c;H0;D3;+0:2]:1-[Cl;H0;D1;+0:1]
null
[]
null
null
1.5
HOUR
A solution of phosphorous oxychloride (3.1 g, 20 mmol) in anhydrous N,N-dimethylformamide (DMF, 14 mL) was added to a suspension of 3-nitro-7-phenylquinolin-4-ol (5.0 g, 18.8 mmol) in 80 mL of DMF over 3 min. The reaction was allowed to stir for 1.5 h and then poured into 250 mL crushed ice. The resulting precipitate w...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol
Aromatic halide
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HCl
CN(C=O)C
null
1.5
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1O>CN(C=O)C>O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8075df8866694ec781accd5f264a85a4
CSCCCN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>>CSCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
ClC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-].CSCCCN>>CSCCCNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-]
[CH3:1][S:2][CH2:3][CH2:4][CH2:5][NH2:6].Cl[c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16](-[c:17]3[cH:18][cH:19][cH:20][cH:21][cH:22]3)[cH:23][cH:24][c:25]12>>[CH3:1][S:2][CH2:3][CH2:4][CH2:5][NH:6][c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16](-[c:17]3[cH:18][cH:19][cH:20][c...
CSCCCN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
CSCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(-c2ccc3cccnc3c2)cc1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
93.3
[{"value": 93.3, "product": "CSCCCNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4—Chloro-3-nitro-7-phenylquinoline (5.3 g, 18.8 mmol) and 3-methylsulfanyl-propylamine (2.17 g, 20.6 mmol) were combined and treated according to the general procedure described in Part E of Example 1. Recrystallization from isopropanol afforded 6.2 g of (3-methylsulfanylpropyl)-(3-nitro-7-phenylquinolin-4-yl)amine as ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HCl
null
null
null
CSCCCN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>>CSCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c0fe02b4047447469750fe6ff08d67db
CSCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12>>CSCCCNc1c(N)cnc2cc(-c3ccccc3)ccc12
CSCCCNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-]>>CSCCCNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)N
O=[N+:9]([O-])[c:8]1[c:7]([NH:6][CH2:5][CH2:4][CH2:3][S:2][CH3:1])[c:23]2[c:12]([n:11][cH:10]1)[cH:13][c:14](-[c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1)[cH:21][cH:22]2>>[CH3:1][S:2][CH2:3][CH2:4][CH2:5][NH:6][c:7]1[c:8]([NH2:9])[cH:10][n:11][c:12]2[cH:13][c:14](-[c:15]3[cH:16][cH:17][cH:18][cH:19][cH:20]3)[cH:21][cH:...
CSCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
CSCCCNc1c(N)cnc2cc(-c3ccccc3)ccc12
null
[Pt]
C1(=CC=CC=C1)C
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(-c2ccc3cccnc3c2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
100
[{"value": 100.0, "product": "CSCCCNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
(3-Methylsulfanylpropyl)-(3-nitro-7-phenylquinolin-4-yl)amine (3.0 g, 8.5 mmol) was hydrogenated in a Parr bottle over Pt/C (0.3 g of 5%) in 42 mL of toluene for 1 h. The reaction mixture was filtered through CELITE filter agent, washed with methanol (100 mL) and CHCl3 (50 mL), and then concentrated to afford 2.75 g of...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1.c1ccccc1
Other
[Pt].C1(=CC=CC=C1)C
null
null
CSCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12>[Pt].C1(=CC=CC=C1)C>CSCCCNc1c(N)cnc2cc(-c3ccccc3)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-db8fbeb70dec4320954face4762c20da
CCCCC(OC)(OC)OC.CSCCCNc1c(N)cnc2cc(-c3ccccc3)ccc12>>CCCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCSC
CSCCCNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)N.C(CCCC)(OC)(OC)OC.Cl.N1=CC=CC=C1>>C(CCC)C=1N(C2=C(C=NC=3C=C(C=CC23)C2=CC=CC=C2)N1)CCCSC
CO[C:5](OC)(OC)[CH2:4][CH2:3][CH2:2][CH3:1].[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][c:12](-[c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)[cH:19][cH:20][c:21]2[c:22]1[NH:23][CH2:24][CH2:25][CH2:26][S:27][CH3:28]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12](-[c:13]4[cH:14][cH:15][cH:16][cH:1...
CCCCC(OC)(OC)OC.CSCCCNc1c(N)cnc2cc(-c3ccccc3)ccc12
CCCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCSC
null
null
C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
8d87c769e65778c9400c7f523e0409ecf0ffad86543cd9fdd6ef4b239323db96
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc(-c2ccc3c(c2)ncc2nc[nH]c23)cc1
C-O-[C;H0;D4;+0:1](-O-C)(-O-C)-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
90.7
[{"value": 90.7, "product": "C(CCC)C=1N(C2=C(C=NC=3C=C(C=CC23)C2=CC=CC=C2)N1)CCCSC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
N4-(3-Methylsulfanylpropyl)-7-phenylquinoline-3,4-diamine (2.75 g, 8.49 mmol), trimethyl orthovalerate (1.7 g, 10 mmol), and pyridine hydrochloride (0.3 g) were dissolved in toluene (28 mL) and heated to reflux for 1.5 h, collecting the volatiles in a Dean—Stark trap. Upon cooling to room temperature, the solvent was r...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HO-
C1(=CC=CC=C1)C
null
1
CCCCC(OC)(OC)OC.CSCCCNc1c(N)cnc2cc(-c3ccccc3)ccc12>C1(=CC=CC=C1)C>CCCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCSC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ed8f627f3e2042acae8a94dcfcac827a
BrBr.CC(C)Cn1cnc2c(N)nc3ccccc3c21>>CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
C(C(C)C)N1C=NC=2C(=NC=3C=CC=CC3C21)N.BrBr>>BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C
Br[Br:16].[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][cH:15][cH:17][c:18]3[c:19]12>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][c:18]3[c:19]12
BrBr.CC(C)Cn1cnc2c(N)nc3ccccc3c21
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
null
null
C(C)(=O)O
Functional Group Interconversion
Bromination
203112cf446e25794477b3f4b62b35c5de4ca920eba5ece53260bfccbd7b9ebb
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc2c(c1)ncc1nc[nH]c12
Br-[Br;H0;D1;+0:1].[#7;a:2]:[c:3]1:[c:4]:[c:5]:[cH;D2;+0:6]:[c:7]:[c:8]:1:[c:9]:[#7;a:10]>>[#7;a:2]:[c:3]1:[c:4]:[c:5]:[c;H0;D3;+0:6](-[Br;H0;D1;+0:1]):[c:7]:[c:8]:1:[c:9]:[#7;a:10]
25.6
[{"value": 25.6, "product": "BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
To a solution of 1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine (10.0 g, 41.6 mmol) in acetic acid (150 mL) was added Br2 (10.0 g, 62.6 mmol), and after 24 h, the resulting solid was collected by filtration and washed with H2O. The orange solid was suspended in a saturated aqueous solution of NaHSO3, after which it was a...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1nc2ccccc2c2[nH]cnc12
c1ccc2ncc3nc[nH]c3c2c1
c1ccc2ncc3nc[nH]c3c2c1
HBr
C(C)(=O)O
null
24
BrBr.CC(C)Cn1cnc2c(N)nc3ccccc3c21>C(C)(=O)O>CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6fe7ec3643804528b4183e666763a9a5
CC(C)(C)c1ccc(B(O)O)cc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21>>CC(C)Cn1cnc2c(N)nc3ccc(-c4ccc(C(C)(C)C)cc4)cc3c21
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C.C(C)(C)(C)C1=CC=C(C=C1)B(O)O>>C(C)(C)(C)C1=CC=C(C=C1)C1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C
OB(O)[c:16]1[cH:17][cH:18][c:19]([C:20]([CH3:21])([CH3:22])[CH3:23])[cH:24][cH:25]1.Br[c:15]1[cH:14][cH:13][c:12]2[n:11][c:9]([NH2:10])[c:8]3[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:28]3[c:27]2[cH:26]1>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][c:15](-[c:16]...
CC(C)(C)c1ccc(B(O)O)cc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
CC(C)Cn1cnc2c(N)nc3ccc(-c4ccc(C(C)(C)C)cc4)cc3c21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
d7a5947e9b277585517ecdc572044d33fd140be4e78d7cb7b0c07b7ea0ac1fa0
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3ncc4nc[nH]c4c3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6](:[c:7]:1):[c:8]:[#7;a:9].O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]):[c:7]:[c:6]:1:[c:8]:[#7;a:9]
null
[]
null
null
null
null
8-Bromo-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and 4-tert-butylbenzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. Recrystallization from isopropanol followed by chromatography on silica gel (7% methanol in CH2Cl2) afforded 8-(4-tert-butylphenyl)-1-isobutyl-1H-imi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccc2ncc3[nH]cnc3c2c1
c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
HBr.B
null
null
null
CC(C)(C)c1ccc(B(O)O)cc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21>>CC(C)Cn1cnc2c(N)nc3ccc(-c4ccc(C(C)(C)C)cc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b5404f3d81c74fca9c293d91f37982f0
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccsc1>>CC(C)Cn1cnc2c(N)nc3ccc(-c4ccsc4)cc3c21
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C.S1C=C(C=C1)B(O)O>>C(C(C)C)N1C=NC=2C(=NC=3C=CC(=CC3C21)C2=CSC=C2)N
Br[c:15]1[cH:14][cH:13][c:12]2[n:11][c:9]([NH2:10])[c:8]3[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:23]3[c:22]2[cH:21]1.OB(O)[c:16]1[cH:17][cH:18][s:19][cH:20]1>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][c:15](-[c:16]4[cH:17][cH:18][s:19][cH:20]4)[cH:21][c:22]...
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccsc1
CC(C)Cn1cnc2c(N)nc3ccc(-c4ccsc4)cc3c21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
0e414bfed961d165ada2a874b7e33ecaa27275bfea10ab6af1b945af426022ad
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1nc2cnc3ccc(-c4ccsc4)cc3c2[nH]1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6](:[c:7]:1):[c:8]:[#7;a:9].O-B(-O)-[c;H0;D3;+0:10]1:[c:11]:[c:12]:[#16;a:13]:[c:14]:1>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10]2:[c:11]:[c:12]:[#16;a:13]:[c:14]:2):[c:7]:[c:6]:1:[c:8]:[#7;a:9]
null
[]
null
null
null
null
8-Bromo-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and thiophene-3-boronic acid were coupled according to the general procedure described in Part J of Example 1. Recrystallization from isopropanol followed by chromatography on silica gel (7% methanol in CH2Cl2) afforded 1-isobutyl-8-(thiophen-3-yl)-1H-imidazo[4,5-c]q...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ncc3[nH]cnc3c2c1.c1ccsc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccsc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccsc1
HBr.B
null
null
null
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccsc1>>CC(C)Cn1cnc2c(N)nc3ccc(-c4ccsc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5f0e7f0c7f184036b62819e4b30b2546
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.COc1ccc(B(O)O)c(OC)c1>>COc1ccc(-c2ccc3nc(N)c4ncn(CC(C)C)c4c3c2)c(OC)c1
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C.COC1=C(C=CC(=C1)OC)B(O)O>>COC1=C(C=CC(=C1)OC)C1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C
Br[c:7]1[cH:8][cH:9][c:10]2[n:11][c:12]([NH2:13])[c:14]3[n:15][cH:16][n:17]([CH2:18][CH:19]([CH3:20])[CH3:21])[c:22]3[c:23]2[cH:24]1.OB(O)[c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:28][c:25]1[O:26][CH3:27]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6](-[c:7]2[cH:8][cH:9][c:10]3[n:11][c:12]([NH2:13])[c:14]4[n:15][cH:16][n:17]([CH2...
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.COc1ccc(B(O)O)c(OC)c1
COc1ccc(-c2ccc3nc(N)c4ncn(CC(C)C)c4c3c2)c(OC)c1
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
53cc9ca90227d2908951e3024c95de9c6c3fb7608365c04a68b45ee49e2f3f42
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3ncc4nc[nH]c4c3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3](:[c:4]:[#7;a:5]):[c:6](:[#7;a:7]):[c:8]:[c:9]:1.O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13](-[#8:14]):[c:15]>>[#7;a:7]:[c:6]1:[c:8]:[c:9]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13](-[#8:14]):[c:15]):[c:2]:[c:3]:1:[c:4]:[#7;a:5]
null
[]
null
null
null
null
8-Bromo-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and 2,4-dimethoxybenzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. Purification by chromatography on silica gel (7% methanol in CH2Cl2) afforded 8-(2,4-dimethoxyphenyl)-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine a...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ncc3[nH]cnc3c2c1.c1ccccc1
c1ccccc1.c1ccc2ncc3[nH]cnc3c2c1
c1ccccc1.c1ccc2ncc3[nH]cnc3c2c1
HBr.B
null
null
null
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.COc1ccc(B(O)O)c(OC)c1>>COc1ccc(-c2ccc3nc(N)c4ncn(CC(C)C)c4c3c2)c(OC)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c043e8636e5b4027bb6bf5e022ac7a37
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1cccnc1>>CC(C)Cn1cnc2c(N)nc3ccc(-c4cccnc4)cc3c21
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C.N1=CC(=CC=C1)B(O)O>>C(C(C)C)N1C=NC=2C(=NC=3C=CC(=CC3C21)C=2C=NC=CC2)N
Br[c:15]1[cH:14][cH:13][c:12]2[n:11][c:9]([NH2:10])[c:8]3[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:24]3[c:23]2[cH:22]1.OB(O)[c:16]1[cH:17][cH:18][cH:19][n:20][cH:21]1>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][c:15](-[c:16]4[cH:17][cH:18][cH:19][n:20][cH:21]4...
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1cccnc1
CC(C)Cn1cnc2c(N)nc3ccc(-c4cccnc4)cc3c21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
5d3693fe08abbbc8184547f1e504a72adf7c4cbfcff89e5476d430c2e1e9dea5
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1cncc(-c2ccc3ncc4nc[nH]c4c3c2)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6](:[c:7]:1):[c:8]:[#7;a:9].O-B(-O)-[c;H0;D3;+0:10]1:[c:11]:[c:12]:[c:13]:[#7;a:14]:[c:15]:1>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10]2:[c:11]:[c:12]:[c:13]:[#7;a:14]:[c:15]:2):[c:7]:[c:6]:1:[c:8]:[#7;a:9]
null
[]
null
null
null
null
8-Bromo-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and pyridine-3-boronic acid were coupled according to the general procedure described in Part J of Example 1. Purification by chromatography on silica gel (7%–10% methanol in CH2Cl2 gradient) afforded 1-isobutyl-8-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine as a...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ncc3[nH]cnc3c2c1.c1ccncc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccncc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccncc1
HBr.B
null
null
null
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1cccnc1>>CC(C)Cn1cnc2c(N)nc3ccc(-c4cccnc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ea48b66e88164bddafa0c996a8011a44
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccccc1>>CC(C)Cn1cnc2c(N)nc3ccc(-c4ccccc4)cc3c21
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C.C1(=CC=CC=C1)B(O)O>>C(C(C)C)N1C=NC=2C(=NC=3C=CC(=CC3C21)C2=CC=CC=C2)N
Br[c:15]1[cH:14][cH:13][c:12]2[n:11][c:9]([NH2:10])[c:8]3[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:24]3[c:23]2[cH:22]1.OB(O)[c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][c:15](-[c:16]4[cH:17][cH:18][cH:19][cH:20][cH:21...
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccccc1
CC(C)Cn1cnc2c(N)nc3ccc(-c4ccccc4)cc3c21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
d7a5947e9b277585517ecdc572044d33fd140be4e78d7cb7b0c07b7ea0ac1fa0
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3ncc4nc[nH]c4c3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6](:[c:7]:1):[c:8]:[#7;a:9].O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]):[c:7]:[c:6]:1:[c:8]:[#7;a:9]
null
[]
null
null
null
null
8-Bromo-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and benzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. Recrystallization from isopropanol followed by recrystallization from methanol afforded 1-isobutyl-8-phenyl-1H-imidazo[4,5-c]quinolin-4-amine as a beige solid, m...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ncc3[nH]cnc3c2c1.c1ccccc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
HBr.B
null
null
null
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccccc1>>CC(C)Cn1cnc2c(N)nc3ccc(-c4ccccc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-81344968fab24210b3c08586347dafa4
CCc1nc2c(N)nc3ccc(Br)cc3c2n1CC(C)C.OB(O)c1ccccc1>>CCc1nc2c(N)nc3ccc(-c4ccccc4)cc3c2n1CC(C)C
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=C(N3CC(C)C)CC.C1(=CC=CC=C1)B(O)O>>C(C)C=1N(C2=C(C(=NC=3C=CC(=CC23)C2=CC=CC=C2)N)N1)CC(C)C
Br[c:12]1[cH:11][cH:10][c:9]2[n:8][c:6]([NH2:7])[c:5]3[n:4][c:3]([CH2:2][CH3:1])[n:22]([CH2:23][CH:24]([CH3:25])[CH3:26])[c:21]3[c:20]2[cH:19]1.OB(O)[c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][c:12](-[c:13]4[cH:14][cH:15][cH:16][cH:17][cH:18]4)[cH:...
CCc1nc2c(N)nc3ccc(Br)cc3c2n1CC(C)C.OB(O)c1ccccc1
CCc1nc2c(N)nc3ccc(-c4ccccc4)cc3c2n1CC(C)C
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
53cc9ca90227d2908951e3024c95de9c6c3fb7608365c04a68b45ee49e2f3f42
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3ncc4nc[nH]c4c3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6](:[c:7]:1):[c:8]:[#7;a:9].O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]>>[#7;a:9]:[c:8]:[c:6]1:[c:7]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]):[c:2]:[c:3]:[c:4]:1:[#7;a:5]
null
[]
null
null
null
null
8-Bromo-2-ethyl-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and benzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. Chromatography on silica gel (5%–7% methanol in CH2Cl2 gradient) afforded 2-ethyl-1-isobutyl-8-phenyl-1H-imidazo[4,5-c]quinolin-4-amine as a white solid,...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ncc3[nH]cnc3c2c1.c1ccccc1
c1ccc2ncc3[nH]cnc3c2c1.c1ccccc1
c1ccc2ncc3[nH]cnc3c2c1.c1ccccc1
HBr.B
null
null
null
CCc1nc2c(N)nc3ccc(Br)cc3c2n1CC(C)C.OB(O)c1ccccc1>>CCc1nc2c(N)nc3ccc(-c4ccccc4)cc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b911d3355fd84051988e9ff9322156c6
CCc1nc2c(N)nc3ccc(Br)cc3c2n1CC(C)C.OB(O)c1cccnc1>>CCc1nc2c(N)nc3ccc(-c4cccnc4)cc3c2n1CC(C)C
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=C(N3CC(C)C)CC.N1=CC(=CC=C1)B(O)O>>C(C)C=1N(C2=C(C(=NC=3C=CC(=CC23)C=2C=NC=CC2)N)N1)CC(C)C
Br[c:12]1[cH:11][cH:10][c:9]2[n:8][c:6]([NH2:7])[c:5]3[n:4][c:3]([CH2:2][CH3:1])[n:22]([CH2:23][CH:24]([CH3:25])[CH3:26])[c:21]3[c:20]2[cH:19]1.OB(O)[c:13]1[cH:14][cH:15][cH:16][n:17][cH:18]1>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7])[n:8][c:9]3[cH:10][cH:11][c:12](-[c:13]4[cH:14][cH:15][cH:16][n:17][cH:18]4)[cH:19...
CCc1nc2c(N)nc3ccc(Br)cc3c2n1CC(C)C.OB(O)c1cccnc1
CCc1nc2c(N)nc3ccc(-c4cccnc4)cc3c2n1CC(C)C
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
bc9cd5af0d1465da413bcba1dea78360c9cd1c2208ec56a2c19fa0e80e6b9c1f
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1cncc(-c2ccc3ncc4nc[nH]c4c3c2)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6](:[c:7]:1):[c:8]:[#7;a:9].O-B(-O)-[c;H0;D3;+0:10]1:[c:11]:[c:12]:[c:13]:[#7;a:14]:[c:15]:1>>[#7;a:9]:[c:8]:[c:6]1:[c:7]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10]2:[c:11]:[c:12]:[c:13]:[#7;a:14]:[c:15]:2):[c:2]:[c:3]:[c:4]:1:[#7;a:5]
null
[]
null
null
null
null
8-Bromo-2-ethyl-1-isobutyl-1H-imidazo[4,5-c]quinolin-4-amine and pyridine-3-boronic acid were coupled according to the general procedure described in Part J of Example 1. Chromatography on silica gel (5%–7% methanol in CH2Cl2 gradient) followed by recrystallization from isopropanol afforded 2-ethyl-1-isobutyl-8-(pyridi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ncc3[nH]cnc3c2c1.c1ccncc1
c1ccc2ncc3[nH]cnc3c2c1.c1ccncc1
c1ccc2ncc3[nH]cnc3c2c1.c1ccncc1
HBr.B
null
null
null
CCc1nc2c(N)nc3ccc(Br)cc3c2n1CC(C)C.OB(O)c1cccnc1>>CCc1nc2c(N)nc3ccc(-c4cccnc4)cc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-42e4e7a533e14cb8940c0844c4da9573
CCCCn1c(COCC)nc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccccc1>>CCCCn1c(COCC)nc2c(N)nc3ccc(-c4ccccc4)cc3c21
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=C(N3CCCC)COCC.C1(=CC=CC=C1)B(O)O>>C(CCC)N1C(=NC=2C(=NC=3C=CC(=CC3C21)C2=CC=CC=C2)N)COCC
Br[c:19]1[cH:18][cH:17][c:16]2[n:15][c:13]([NH2:14])[c:12]3[n:11][c:6]([CH2:7][O:8][CH2:9][CH3:10])[n:5]([CH2:4][CH2:3][CH2:2][CH3:1])[c:28]3[c:27]2[cH:26]1.OB(O)[c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1>>[CH3:1][CH2:2][CH2:3][CH2:4][n:5]1[c:6]([CH2:7][O:8][CH2:9][CH3:10])[n:11][c:12]2[c:13]([NH2:14])[n:15][c:16]3[cH...
CCCCn1c(COCC)nc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccccc1
CCCCn1c(COCC)nc2c(N)nc3ccc(-c4ccccc4)cc3c21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
d7a5947e9b277585517ecdc572044d33fd140be4e78d7cb7b0c07b7ea0ac1fa0
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3ncc4nc[nH]c4c3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6](:[c:7]:1):[c:8]:[#7;a:9].O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]):[c:7]:[c:6]:1:[c:8]:[#7;a:9]
null
[]
null
null
null
null
8-Bromo-1-butyl-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-4-amine and benzeneboronic acid were coupled according to the general procedure described in Part J of Example 1. Chromatography on silica gel (10% methanol in CH2Cl2) followed by recrystallization from isopropanol afforded 1-butyl-2-ethoxymethyl-8-phenyl-1H-imid...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ncc3[nH]cnc3c2c1.c1ccccc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
HBr.B
null
null
null
CCCCn1c(COCC)nc2c(N)nc3ccc(Br)cc3c21.OB(O)c1ccccc1>>CCCCn1c(COCC)nc2c(N)nc3ccc(-c4ccccc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c28838e1bbc145a798736594e16b04cc
CCCCn1c(COCC)nc2c(N)nc3ccc(Br)cc3c21.OB(O)c1cccnc1>>CCCCn1c(COCC)nc2c(N)nc3ccc(-c4cccnc4)cc3c21
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=C(N3CCCC)COCC.N1=CC(=CC=C1)B(O)O>>C(CCC)N1C(=NC=2C(=NC=3C=CC(=CC3C21)C=2C=NC=CC2)N)COCC
Br[c:19]1[cH:18][cH:17][c:16]2[n:15][c:13]([NH2:14])[c:12]3[n:11][c:6]([CH2:7][O:8][CH2:9][CH3:10])[n:5]([CH2:4][CH2:3][CH2:2][CH3:1])[c:28]3[c:27]2[cH:26]1.OB(O)[c:20]1[cH:21][cH:22][cH:23][n:24][cH:25]1>>[CH3:1][CH2:2][CH2:3][CH2:4][n:5]1[c:6]([CH2:7][O:8][CH2:9][CH3:10])[n:11][c:12]2[c:13]([NH2:14])[n:15][c:16]3[cH:...
CCCCn1c(COCC)nc2c(N)nc3ccc(Br)cc3c21.OB(O)c1cccnc1
CCCCn1c(COCC)nc2c(N)nc3ccc(-c4cccnc4)cc3c21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
5d3693fe08abbbc8184547f1e504a72adf7c4cbfcff89e5476d430c2e1e9dea5
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1cncc(-c2ccc3ncc4nc[nH]c4c3c2)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6](:[c:7]:1):[c:8]:[#7;a:9].O-B(-O)-[c;H0;D3;+0:10]1:[c:11]:[c:12]:[c:13]:[#7;a:14]:[c:15]:1>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10]2:[c:11]:[c:12]:[c:13]:[#7;a:14]:[c:15]:2):[c:7]:[c:6]:1:[c:8]:[#7;a:9]
null
[]
null
null
null
null
8-Bromo-1-butyl-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-4-amine and pyridine-3-boronic acid were coupled according to the general procedure described in Part J of Example 1. Chromatography on silica gel (8%–10% methanol in CH2Cl2 gradient) followed by recrystallization from isopropanol (3×) and chromatography as above...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ncc3[nH]cnc3c2c1.c1ccncc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccncc1
c1ccc2ncc3nc[nH]c3c2c1.c1ccncc1
HBr.B
null
null
null
CCCCn1c(COCC)nc2c(N)nc3ccc(Br)cc3c21.OB(O)c1cccnc1>>CCCCn1c(COCC)nc2c(N)nc3ccc(-c4cccnc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5d4c45ec99c44e3195ba265c9d851613
CC(C)(C)[Si](C)(C)OCc1cncc(Br)c1.CC(C)OB(OC(C)C)OC(C)C.[Li][CH2]CCC.[NH4+]>>CC(C)(C)[Si](C)(C)OCc1cncc(B(O)O)c1.CC(C)(C)[Si](C)(C)OCc1cncc(Br)c1
[Cl-].[NH4+].BrC=1C=NC=C(C1)CO[Si](C)(C)C(C)(C)C.B(OC(C)C)(OC(C)C)OC(C)C.C(CCC)[Li]>>BrC=1C=NC=C(C1)CO[Si](C)(C)C(C)(C)C.[Si](C)(C)(C(C)(C)C)OCC=1C=C(C=NC1)B(O)O
[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([CH3:6])([CH3:7])[O:8][CH2:9][c:10]1[cH:11][n:12][cH:31][c:32]([Br:33])[cH:34]1.C([O:16][B:15]([O:17][CH:20]([CH3:21])[CH3:22])[O:26][CH:27]([CH3:19])[CH3:28])([CH3:24])[CH3:25].[Li][CH2:13][CH2:14][CH2:18][CH3:29].[NH4+:30]>>[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([CH3:6])([CH3:7])[O:...
CC(C)(C)[Si](C)(C)OCc1cncc(Br)c1.CC(C)OB(OC(C)C)OC(C)C.[Li][CH2]CCC.[NH4+]
CC(C)(C)[Si](C)(C)OCc1cncc(B(O)O)c1.CC(C)(C)[Si](C)(C)OCc1cncc(Br)c1
null
null
C1CCOC1.O
Aromatic Heterocycle Formation
OtherReaction
760ffe1126c708fb30f687132fd5f9d9d71261d64559658713a72c3632875204
05caca3ab5e3f1ac57dd8889f11d62a26dead3dbc27832571298c14785df3016
c1ccncc1.c1ccncc1
[#8:1]-[C:2]-[c;H0;D3;+0:3]1:[c:4]:[n;H0;D2;+0:5]:[cH;D2;+0:6]:[c:7](-[Br;D1;H0:8]):[cH;D2;+0:9]:1.[C;D1;H3:10]-[CH;D3;+0:11](-[C;D1;H3:12])-[O;H0;D2;+0:13]-[B;H0;D3;+0:14](-[O;H0;D2;+0:15]-C(-[CH3;D1;+0:16])-[CH3;D1;+0:17])-[O;H0;D2;+0:18]-[CH;D3;+0:19](-[CH3;D1;+0:20])-[CH3;D1;+0:21].[CH3;D1;+0:22]-[CH2;D2;+0:23]-[CH...
143.4
[{"value": 143.4, "product": "[Si](C)(C)(C(C)(C)C)OCC=1C=C(C=NC1)B(O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-20
CELSIUS
30
MINUTE
3-Bromo-5-(tert-butyldimethylsilanyloxymethyl)pyridine was prepared according to the published procedure (Zhang, N. et al, J. Med. Chem., 45, 2832–2840 (2002)). Under a nitrogen atmosphere, a solution of 3-bromo-5-(tert-butyldimethylsilanyloxymethyl)pyridine (28.70 g, 94.94 mmol) and triisopropyl borate (26.3 mL, 114 m...
10.6084/m9.figshare.5104873.v1
null
Alkyl lithium
Boronic acid.TMS ether protective group
c1ccncc1
c1ccncc1.c1ccncc1
c1ccncc1.c1ccncc1
Li
C1CCOC1.O
-20
0.5
CC(C)(C)[Si](C)(C)OCc1cncc(Br)c1.CC(C)OB(OC(C)C)OC(C)C.[Li][CH2]CCC.[NH4+]>C1CCOC1.O>CC(C)(C)[Si](C)(C)OCc1cncc(B(O)O)c1.CC(C)(C)[Si](C)(C)OCc1cncc(Br)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ce608b941e714b91967ecf915812fdb8
CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccccc4)cc3c21>>CC(C)Cn1cnc2c(N)nc3ccc(CCc4ccccc4)cc3c21
CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)C=CC2=CC=CC=C2)N)C>>CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)CCC2=CC=CC=C2)N)C
[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][c:15]([CH:16]=[CH:17][c:18]4[cH:19][cH:20][cH:21][cH:22][cH:23]4)[cH:24][c:25]3[c:26]12>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[c:9]([NH2:10])[n:11][c:12]3[cH:13][cH:14][c:15]([CH2:16][CH2:17][c:18]4[cH:19][cH:2...
CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccccc4)cc3c21
CC(C)Cn1cnc2c(N)nc3ccc(CCc4ccccc4)cc3c21
null
[Pd]
C(C)O
Reduction
Hydrogenation (double to single)
0bc3968b35f0839c230afb4215314da278abd4e1f10e42ec3012c5512de49ea5
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1ccc(CCc2ccc3ncc4nc[nH]c4c3c2)cc1
[c:1]:[c:2](-[CH;D2;+0:3]=[CH;D2;+0:4]-[c:5](:[c:6]):[c:7]):[c:8]>>[c:1]:[c:2](-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[c:5](:[c:6]):[c:7]):[c:8]
21.8
[{"value": 21.8, "product": "CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)CCC2=CC=CC=C2)N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 1-(2-methylpropyl)-8-styryl-1H-imidazo[4,5-c]quinolin-4-amine (1.37 g, 4.00 mmol) in ethanol (40 mL) was added to a Parr vessel charged with 10% palladium on carbon (137 mg). The reaction was placed under hydrogen pressure (40 psi, 2.8×105 Pa) for six days. The reaction mixture was filtered through a laye...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
null
[Pd].C(C)O
null
null
CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccccc4)cc3c21>[Pd].C(C)O>CC(C)Cn1cnc2c(N)nc3ccc(CCc4ccccc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-264de42745e6441b818c0fd73a192dd5
CC(C)(O)CN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
C(C)N(CC)CC.BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.NCC(C)(O)C>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC(C)(O)C
[CH3:1][C:2]([CH3:3])([OH:4])[CH2:5][NH2:6].Cl[c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16]([Br:17])[cH:18][cH:19][c:20]12>>[CH3:1][C:2]([CH3:3])([OH:4])[CH2:5][NH:6][c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16]([Br:17])[cH:18][cH:19][c:20]12
CC(C)(O)CN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
null
null
ClCCl
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2ncccc2c1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
78.5
[{"value": 78.5, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC(C)(O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
8
HOUR
Triethylamine (17.35 mL, 124 mmol) was added to a solution of 7-bromo-4-chloro-3-nitroquinoline (29.84 g, 104 mmol) in dichloromethane (253 mL), and the reaction was cooled to 0° C. 1-Amino-2-methylpropan-2-ol (10.17 g, 114 mmol) was added dropwise, and then the reaction was allowed to warm to ambient temperature and s...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
ClCCl
0
8
CC(C)(O)CN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>ClCCl>CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1a6beef3a19343c4ac3cbf90e4bc2e18
CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC(C)(O)C>>NC=1C=NC2=CC(=CC=C2C1NCC(C)(O)C)Br
O=[N+:9]([O-])[c:8]1[c:7]([NH:6][CH2:5][C:2]([CH3:1])([CH3:3])[OH:4])[c:18]2[c:12]([n:11][cH:10]1)[cH:13][c:14]([Br:15])[cH:16][cH:17]2>>[CH3:1][C:2]([CH3:3])([OH:4])[CH2:5][NH:6][c:7]1[c:8]([NH2:9])[cH:10][n:11][c:12]2[cH:13][c:14]([Br:15])[cH:16][cH:17][c:18]12
CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12
null
[Pt]
C(C)#N
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2ncccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
85.7
[{"value": 85.7, "product": "NC=1C=NC2=CC(=CC=C2C1NCC(C)(O)C)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 1-(7-bromo-3-nitroquinolin-4-ylamino)-2-methylpropan-2-ol (27.78 g, 81.66 mmol) in acetonitrile (1.2 L) was added to a Parr vessel charged with 5% platinum on carbon (0.84 g), and the reaction was placed under hydrogen pressure (50 psi, 3.4×105 Pa) for two days. The reaction mixture was filtered through a...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C(C)#N
null
null
CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>[Pt].C(C)#N>CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-408b6bd98e6c455a89225c1e8c5e9238
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl>>CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCC(C)(C)O
NC=1C=NC2=CC(=CC=C2C1NCC(C)(O)C)Br.C(C)OCC(=O)Cl>>BrC1=CC=C2C(=C(C=NC2=C1)NC(COCC)=O)NCC(C)(C)O
[NH2:7][c:8]1[cH:9][n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[c:18]1[NH:19][CH2:20][C:21]([CH3:22])([CH3:23])[OH:24].Cl[C:5]([CH2:4][O:3][CH2:2][CH3:1])=[O:6]>>[CH3:1][CH2:2][O:3][CH2:4][C:5](=[O:6])[NH:7][c:8]1[cH:9][n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[c:18]1[NH:19][CH2:20][C:21]([CH3...
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl
CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCC(C)(C)O
null
null
ClCCl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc2ncccc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#8:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]:[#7;a:9]:[c:10]>>[#8:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]:[#7;a:9]:[c:10]
null
[]
null
null
8
HOUR
A solution of 1-(3-amino-7-bromoquinolin-4-ylamino)-2-methylpropan-2-ol (158.19 g, 0.510 mol) in dichloromethane (1.2 L) was cooled to 0° C. Ethoxyacetyl chloride (62.50 g, 0.510 mol) was added dropwise, and then the reaction was allowed to warm to ambient temperature and stirred overnight. A precipitate formed and was...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2ncccc2c1
HCl
ClCCl
null
8
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl>ClCCl>CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCC(C)(C)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2ad48777879c49898552a1d3c495787b
CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCC(C)(C)O>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
[OH-].[Na+].BrC1=CC=C2C(=C(C=NC2=C1)NC(COCC)=O)NCC(C)(C)O>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)COCC
O=[C:5]([CH2:4][O:3][CH2:2][CH3:1])[NH:6][c:7]1[cH:8][n:9][c:10]2[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]2[c:17]1[NH:18][CH2:19][C:20]([CH3:21])([CH3:22])[OH:23]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][C:20]([CH3:21])([CH3:22])[OH...
CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCC(C)(C)O
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
null
null
O.C(C)O
Aromatic Heterocycle Formation
OtherReaction
a6a1d4e36f45189361154011b48477e6e08494aa3d520e5d656bee23ebaa3d72
71fdeda1d5481ba7466e825735d29b5ffca597c091e9548c43a80a0aea31b8a0
c1ccc2c(c1)ncc1nc[nH]c12
O=[C;H0;D3;+0:1](-[C:2]-[#8:3])-[NH;D2;+0:4]-[c:5]1:[c:6]:[#7;a:7]:[c:8]:[c:9]:[c:10]:1-[NH;D2;+0:11]-[C:12]-[C:13]>>[#8:3]-[C:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:4]:[c:5]2:[c:6]:[#7;a:7]:[c:8]:[c:9]:[c:10]:2:[n;H0;D3;+0:11]:1-[C:12]-[C:13]
49.3
[{"value": 49.3, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of sodium hydroxide (25 g, 0.625 mol) in water (205 mL) was added to a solution of N-[7-bromo-4-(2-hydroxy-2-methylpropylamino)quinolin-3-yl]-2-ethoxyacetamide (170.88 g, 0.431 mol) in ethanol (700 mL), and the reaction was heated at reflux under a nitrogen atmosphere for two hours. Upon cooling the reaction...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
HO-
O.C(C)O
null
null
CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCC(C)(C)O>O.C(C)O>CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-db1f569af9f74fb396843cd058260599
CCI.CN(C)C=O.C[Si](C)(C)[N-][Si](C)(C)C.OCc1cncc(Br)c1>>CCOCc1cncc(Br)c1.OCc1cncc(Br)c1
BrC=1C=C(C=NC1)CO.ICC.CN(C)C=O.C[Si](C)(C)[N-][Si](C)(C)C.[Na+]>>BrC=1C=C(C=NC1)CO.BrC=1C=NC=C(C1)COCC
I[CH2:2][CH3:1].[CH3:6][N:7]([CH:13]=[O:12])[CH3:17].C[Si]([N-][Si](C)(C)[CH3:20])([CH3:14])[CH3:18].[OH:3][CH2:4][c:5]1[cH:11][c:9]([Br:10])[cH:8][n:16][cH:15]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[cH:6][n:7][cH:8][c:9]([Br:10])[cH:11]1.[OH:12][CH2:13][c:14]1[cH:15][n:16][cH:17][c:18]([Br:19])[cH:20]1
CCI.CN(C)C=O.C[Si](C)(C)[N-][Si](C)(C)C.OCc1cncc(Br)c1
CCOCc1cncc(Br)c1.OCc1cncc(Br)c1
null
null
C1CCOC1.[Cl-].[Na+].O
Aromatic Heterocycle Formation
OtherReaction
fc04c4ae40dd12bafa2c8a65fc824c07c7ff335d0d21f5e538d55613c2190bc4
e808c4eb1c226ff0e8ce0911837bdf7c02e220c858f4a3b662b483795bf854c7
c1ccncc1.c1ccncc1
C-[Si](-[CH3;D1;+0:1])(-[CH3;D1;+0:2])-[N-]-[Si](-C)(-C)-[CH3;D1;+0:3].I-[CH2;D2;+0:4]-[C;D1;H3:5].[Br;D1;H0:6]-[c:7]1:[c:8]:[c;H0;D3;+0:9](-[C:10]-[OH;D1;+0:11]):[cH;D2;+0:12]:[n;H0;D2;+0:13]:[cH;D2;+0:14]:1.[CH3;D1;+0:15]-[N;H0;D3;+0:16](-[CH3;D1;+0:17])-[CH;D2;+0:18]=[O;H0;D1;+0:19]>>[Br;D1;H0:20]-[c;H0;D3;+0:2]1:[c...
120.4
[{"value": 120.4, "product": "BrC=1C=NC=C(C1)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
(5-Bromopyridin-3-yl)methanol was prepared according to the published procedure (Zhang, N. et al, J. Med. Chem., 45, 2832–2840 (2002)). A solution of (5-bromopyridin-3-yl)methanol (7.39 g, 39.3 mmol) in THF was cooled to 0° C. Sodium bis(trimethylsilyl)amide (39.3 mL of a 1.0 M solution in THF) was added, and the react...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Tertiary amide.Primary alcohol.Silyl protective group.Silyl protective group
Aromatic halide.Ether.Primary alcohol
c1ccncc1
c1ccncc1.c1ccncc1
c1ccncc1.c1ccncc1
HI
C1CCOC1.[Cl-].[Na+].O
null
0.333333
CCI.CN(C)C=O.C[Si](C)(C)[N-][Si](C)(C)C.OCc1cncc(Br)c1>C1CCOC1.[Cl-].[Na+].O>CCOCc1cncc(Br)c1.OCc1cncc(Br)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-395c3b609d4b49cb8302ff782ff91fc2
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.COCCC(=O)Cl>>COCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
NC=1C=NC2=CC(=CC=C2C1NCC(C)(O)C)Br.COCCC(=O)Cl>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)CCOC
[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]2[c:17]1[NH:18][CH2:19][C:20]([CH3:21])([CH3:22])[OH:23].O=[C:5](Cl)[CH2:4][CH2:3][O:2][CH3:1]>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][C:20]([CH3:21])([CH3:22]...
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.COCCC(=O)Cl
COCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
null
null
null
Aromatic Heterocycle Formation
OtherReaction
101a087a520f159c722ba3d78ed38f5c3c1cf154206e5edbeb1e6397c929560f
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
37.6
[{"value": 37.6, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)CCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The method described in Part A of Example 9 was used to react 1-(3-amino-7-bromoquinolin-4-ylamino)-2-methylpropan-2-ol (29.0 g, 93.5 mmol) with 3-methoxypropionyl chloride (11.5 g, 93.5 mmol). The crude product was recrystallized from 2:1 ethyl acetate:hexane and then purified by flash column chromatography on silica ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
HCl
null
null
null
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.COCCC(=O)Cl>>COCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-02ae989cd742463bb79e291df0179b6e
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCOC(CC)(OCC)OCC>>CCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
C(CC)(OCC)(OCC)OCC.NC=1C=NC2=CC(=CC=C2C1NCC(C)(O)C)Br>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)CC
[NH2:4][c:5]1[cH:6][n:7][c:8]2[cH:9][c:10]([Br:11])[cH:12][cH:13][c:14]2[c:15]1[NH:16][CH2:17][C:18]([CH3:19])([CH3:20])[OH:21].CCO[C:3](OCC)(OCC)[CH2:2][CH3:1]>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[cH:6][n:7][c:8]3[cH:9][c:10]([Br:11])[cH:12][cH:13][c:14]3[c:15]2[n:16]1[CH2:17][C:18]([CH3:19])([CH3:20])[OH:21]
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCOC(CC)(OCC)OCC
CCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
null
Cl.N1=CC=CC=C1
C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
8d87c769e65778c9400c7f523e0409ecf0ffad86543cd9fdd6ef4b239323db96
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc2c(c1)ncc1nc[nH]c12
C-C-O-[C;H0;D4;+0:1](-O-C-C)(-O-C-C)-[C:2]-[C;D1;H3:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C;D1;H3:3]
74.9
[{"value": 74.9, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Triethyl orthopropionate (12.9 g, 73.2 mmol) and pyridine hydrochloride (220 mg) were added to a solution of 1-(3-amino-7-bromoquinolin-4-ylamino)-2-methylpropan-2-ol (22.1 g, 70.6 mmol) in anhydrous toluene (300 mL), and the reaction was heated at reflux for three hours. The reaction was allowed to cool to ambient tem...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
HO-
Cl.N1=CC=CC=C1.C1(=CC=CC=C1)C
null
8
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCOC(CC)(OCC)OCC>Cl.N1=CC=CC=C1.C1(=CC=CC=C1)C>CCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-27157f317997486caae24016ad7f66b9
COCCC(=O)Cl.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.c1cncc(B2OCCCO2)c1>>COCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(C)C.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C
B1(OCCCO1)C2=CN=CC=C2.COCCC(=O)Cl.BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCOC>>BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCOC.COCCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC(C)C
O=[C:36](Cl)[CH2:32][CH2:33][O:30][CH3:29].[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:38][c:39]3[cH:40][c:41]([Br:42])[cH:43][cH:44][c:45]3[c:23]2[n:24]1[CH2:25][CH:26]([CH3:11])[CH3:28].O1B([c:14]2[cH:15][cH:16][cH:17][n:18][cH:19]2)O[CH2:21][CH2:13][CH2:12]1>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7...
COCCC(=O)Cl.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.c1cncc(B2OCCCO2)c1
COCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(C)C.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C
null
null
null
Aromatic Heterocycle Formation
OtherReaction
22eeef8d2867cd46bc9b0334f40a3c9f431e063346a181dfca12853c8e7a4524
8a03c963f30a59ff1b31f4b4b4c7ea5336540579bac90f8751e8dead2fccdf88
c1ccc2c(c1)ncc1nc[nH]c12.c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Cl-[C;H0;D3;+0:1](=O)-[CH2;D2;+0:2]-[CH2;D2;+0:3]-[O;H0;D2;+0:4]-[C;D1;H3:5].O1-[CH2;D2;+0:6]-[CH2;D2;+0:7]-[CH2;D2;+0:8]-O-B-1-[c;H0;D3;+0:9]1:[c:10]:[c:11]:[c:12]:[#7;a:13]:[c:14]:1.[C:15]-[c:16]1:[#7;a:17]:[c:18]2:[c;H0;D3;+0:19](:[#7;a:20]:1-[C:21]-[CH;D3;+0:22](-[C;D1;H3:23])-[CH3;D1;+0:24]):[c;H0;D3;+0:25](:[c:26...
null
[]
null
null
null
null
7-Bromo-2-(2-methoxyethyl)-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine was prepared according to the procedures described in Parts A and B of Example 9 using methoxypropanoyl chloride instead of ethoxyacetyl chloride. 7-Bromo-2-(2-methoxyethyl)-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine was coupled w...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether
Ether.Primary amine
c1ccc2c(c1)ncc1[nH]cnc12.B1OCCCO1.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.c1ccc2c(c1)ncc1[nH]cnc12
B
null
null
null
COCCC(=O)Cl.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C.c1cncc(B2OCCCO2)c1>>COCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(C)C.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-89710722be634071be32e1e455135d49
CC(C)(C)[Si](C)(C)OCc1cncc(B(O)O)c1.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C>>COCCc1nc2c(N)nc3cc(-c4cncc(CO)c4)ccc3c2n1CC(C)C
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCOC.[Si](C)(C)(C(C)(C)C)OCC=1C=C(C=NC1)B(O)O>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC(C)C)CCOC)C=2C=C(C=NC2)CO
CC(C)(C)[Si](C)(C)[O:20][CH2:19][c:18]1[cH:17][n:16][cH:15][c:14](B(O)O)[cH:21]1.Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][CH2:3][O:2][CH3:1])[n:26]([CH2:27][CH:28]([CH3:29])[CH3:30])[c:25]3[c:24]2[cH:23][cH:22]1>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:...
CC(C)(C)[Si](C)(C)OCc1cncc(B(O)O)c1.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C
COCCc1nc2c(N)nc3cc(-c4cncc(CO)c4)ccc3c2n1CC(C)C
null
null
null
C-C Coupling
OtherReaction
7e8e494468fec989e28e71c5f1c2fd0a84fe5aaf7514dc78f19f4105e118149d
a06ef17bc21d1c24abf9db7738e014318bfc7beb94875100ee37eca1fd591678
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:13]-[C:14]-[c:15]1:[c:16]:[#7;a:17]:[c:18]:[c;H0;D3;+0:19](-B(-O)-O):[c:20]:1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:19]3:[c:18]:[#7;a:17]:[c:16]:[c:...
null
[]
null
null
null
null
7-Bromo-2-(2-methoxyethyl)-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine was coupled with 5-(tert-butyldimethylsilanyloxymethyl)pyridine-3-boronic acid according to the method described in Examples 118–121. The reaction was heated at reflux for 2.25 hours, and the work-up procedure described in Part F of Example...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid.TMS ether protective group
Primary alcohol
c1ccncc1.c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HBr.B
null
null
null
CC(C)(C)[Si](C)(C)OCc1cncc(B(O)O)c1.COCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C>>COCCc1nc2c(N)nc3cc(-c4cncc(CO)c4)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ab593658aea3483d87d1ad57cc97e475
CC(C)(C)OC(=O)NCCCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>CC(C)(C)OC(=O)NCCCCNc1c(N)cnc2cc(Br)ccc12
S(=O)([O-])S(=O)[O-].[Na+].[Na+].C([O-])([O-])=O.[K+].[K+].C(C)(C)(C)OC(NCCCCNC1=C(C=NC2=CC(=CC=C12)Br)[N+](=O)[O-])=O>>C(C)(C)(C)OC(NCCCCNC1=C(C=NC2=CC(=CC=C12)Br)N)=O
O=[N+:16]([O-])[c:15]1[c:14]([NH:13][CH2:12][CH2:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[c:25]2[c:19]([n:18][cH:17]1)[cH:20][c:21]([Br:22])[cH:23][cH:24]2>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:13][c:14]1[c:15]([NH2:16])[cH:17][n:18][c...
CC(C)(C)OC(=O)NCCCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
CC(C)(C)OC(=O)NCCCCNc1c(N)cnc2cc(Br)ccc12
null
[Br-].[Br-].C(C)[N+]1=CC=C(C=C1)C1=CC=[N+](C=C1)CC
ClCCl.O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2ncccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
99
[{"value": 99.0, "product": "C(C)(C)(C)OC(NCCCCNC1=C(C=NC2=CC(=CC=C12)Br)N)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of sodium hydrosulfite (43.35 g, 249 mmol) and potassium carbonate (38.28 g, 277 mmol) in water (300 mL) was added to a mixture of tert-butyl[4-(7-bromo-3-nitroquinolin-4-ylamino)butyl]carbamate (24.3 g, 55.3 mmol) and 1,1′-diethyl-4,4′-bipyridinium dibromide (1.03 g, 2.76 mmol) in dichloromethane (368 mL) a...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Br-].[Br-].C(C)[N+]1=CC=C(C=C1)C1=CC=[N+](C=C1)CC.ClCCl.O
null
8
CC(C)(C)OC(=O)NCCCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>[Br-].[Br-].C(C)[N+]1=CC=C(C=C1)C1=CC=[N+](C=C1)CC.ClCCl.O>CC(C)(C)OC(=O)NCCCCNc1c(N)cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7fc97130c44c4ab6862ae4441f6c5ab3
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCN
Cl.C(C)(C)(C)OC(NCCCCN1C(=NC=2C=NC=3C=C(C=CC3C21)Br)COCC)=O>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCN)COCC
CC(C)(C)OC(=O)[NH:23][CH2:22][CH2:21][CH2:20][CH2:19][n:18]1[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]21>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][CH2:21][CH...
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCN
null
null
C(C)O
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2c(c1)ncc1nc[nH]c12
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
93.9
[{"value": 93.9, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCN)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Concentrated hydrochloric acid (15.6 mL, 0.194 mol) was added to a solution of tert-butyl[4-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)butyl]carbamate (23.2 g, 48 mmol) in ethanol, and the reaction was heated at reflux for 20 minutes. A precipitate formed, and the reaction was allowed to cool to ambient tem...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2c(c1)ncc1[nH]cnc12
HO-
C(C)O
null
null
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C>C(C)O>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCN
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5987f786235c405b8c7944aed4cb6087
CC(C)(C)OC(=O)NCCCCNc1c(N)cnc2cc(Br)ccc12.CCCc1nc2cnc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C>>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C
C(C)(C)(C)OC(NCCCCNC1=C(C=NC2=CC(=CC=C12)Br)N)=O.C(CCC)(=O)Cl.C(C)(C)(C)OC(NCCCCN1C(=NC=2C=NC=3C=C(C=CC3C21)Br)CCC)=O>>C(C)(C)(C)OC(NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)CCC)=O
CC(C)(C)OC(=O)NCCCCNc1c2ccc(Br)cc2nc[c:7]1[NH2:8].c1[c:6]2[n:5][c:4]([CH2:3][CH2:2][CH3:1])[n:18]([CH2:19][CH2:20][CH2:21][CH2:22][NH:23][C:24](=[O:25])[O:26][C:27]([CH3:28])([CH3:29])[CH3:30])[c:17]2[c:16]2[c:10]([n:9]1)[cH:11][c:12]([Br:13])[cH:14][cH:15]2>>[CH3:1][CH2:2][CH2:3][c:4]1[n:5][c:6]2[c:7]([NH2:8])[n:9][c:...
CC(C)(C)OC(=O)NCCCCNc1c(N)cnc2cc(Br)ccc12.CCCc1nc2cnc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C
null
null
null
Miscellaneous
OtherReaction
fb10f8a85b614d4ce380f86b388af3e848211ee5aa02ec6cfb04b5e4266c42a3
b8bf564d25195599ebf41896df823cfdb0e024456b80eb954e12ecfad8055d4d
c1ccc2c(c1)ncc1nc[nH]c12
Br-c1:c:c:c2:c(-N-C-C-C-C-N-C(=O)-O-C(-C)(-C)-C):[c;H0;D3;+0:1](-[N;D1;H2:2]):c:n:c:2:c:1.[C:3]-[#7;a:4]1:[c:5]:[#7;a:6]:[c;H0;D3;+0:7]2:c:[n;H0;D2;+0:8]:[c:9](:[c:10]):[c:11]:[c:12]:1:2>>[C:3]-[#7;a:4]1:[c:5]:[#7;a:6]:[c;H0;D3;+0:7]2:[c:12]:1:[c:11]:[c:9](:[c:10]):[n;H0;D2;+0:8]:[c;H0;D3;+0:1]:2-[N;D1;H2:2]
null
[]
null
null
null
null
tert-Butyl[4-(3-amino-7-bromoquinolin-4-ylamino)butyl]carbamate was treated with butyryl chloride and cyclized according to the methods described in Part C and D of Examples 125–135. The resulting product, tert-butyl[4-(7-bromo-2-propyl-1H-imidazo[4,5-c]quinolin-1-yl)butyl]carbamate was oxidized and aminated according ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ether.Secondary amine.Boc
null
c1ccc2ncccc2c1.c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
HBr
null
null
null
CC(C)(C)OC(=O)NCCCCNc1c(N)cnc2cc(Br)ccc12.CCCc1nc2cnc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C>>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-64210660bf0948f5bd7e03f4a92c51a0
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1COC(C)(C)O1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(O)CO
Cl.CC1(OCC(O1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)C>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC(CO)O)COCC)C=2C=NC=CC2
CC1(C)[O:27][CH:26]([CH2:25][n:24]2[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]3[c:8]([NH2:9])[n:10][c:11]4[cH:12][c:13](-[c:14]5[cH:15][cH:16][cH:17][n:18][cH:19]5)[cH:20][cH:21][c:22]4[c:23]32)[CH2:28][O:29]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][cH...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1COC(C)(C)O1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(O)CO
null
null
C1CCOC1
Deprotection
Acetal hydrolysis to diol
5f7e1daa6b91d1ca6716348acae46f804565b19cb8bd8a05be2ed6c083743e87
d0de49ebcb43eafba55a762f6d5237c53d7a87b3a882d6753f793a17a3c3a120
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
C-C1(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])-[C:4]-[O;H0;D2;+0:5]-1>>[C:3]-[C:2](-[OH;D1;+0:1])-[C:4]-[OH;D1;+0:5]
89.6
[{"value": 89.6, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC(CO)O)COCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Hydrochloric acid (12 mL of 1 N) was added to a solution of 1-[(2,2-dimethyl-1,3-dioxolan-4-yl)methyl]-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine (0.75 g, 1.73 mmol) in THF, and the reaction was stirred overnight at ambient temperature. The THF was removed under reduced pressure, and 1% aqueous s...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Primary alcohol.Secondary alcohol
C1COCO1
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
Other
C1CCOC1
null
8
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1COC(C)(C)O1>C1CCOC1>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(O)CO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-808e43500c7f426ea4c6f20f0b65c5de
COCCCN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>COCCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.COCCCN>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCOC
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][NH2:6].Cl[c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16]([Br:17])[cH:18][cH:19][c:20]12>>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][NH:6][c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16]([Br:17])[cH:18][cH:19][c:20]12
COCCCN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
COCCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2ncccc2c1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
94.2
[{"value": 94.2, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7-Bromo-4-chloro-3-nitroquinoline (29.54 g, 102.7 mmol) was reacted with 3-methoxy propyl amine (10.07 g, 113.0 mmol) according to the method described in Part A of Examples 125–135 to provide 32.9 g of (7-bromo-3-nitroquinolin-4-yl)-(3-methoxypropyl)amine as a yellow solid. The product was not recrystallized. Conditio...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
null
null
null
COCCCN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>COCCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-04d591006e5b432d8b0818bceb09fc67
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2CCN(CC2)C(=O)OC(C)(C)C)COCC)Br.B1(OCCCO1)C2=CN=CC=C2>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2CCN(CC2)C(=O)OC(C)(C)C)COCC)C=2C=NC=CC2
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:24]([CH2:25][CH:26]4[CH2:27][CH2:28][N:29]([C:30](=[O:31])[O:32][C:33]([CH3:34])([CH3:35])[CH3:36])[CH2:37][CH2:38]4)[c:23]3[c:22]2[cH:21][cH:20]1.C1COB([c:14]2[cH:15][cH:16][cH:17][n:18][cH:19]2)OC1>>[CH3:1][CH2:2][O:3][CH2:4][c:...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1.c1cncc(B2OCCCO2)c1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
null
null
null
C-C Coupling
Suzuki coupling with boronic esters
2cd1cbe6f17c98cb5223a75d20dfc144a6eae8461c4fe8a7e9cc4bc7ecadb166
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1cncc(-c2ccc3c(c2)ncc2ncn(CC4CCNCC4)c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.C1-C-O-B(-[c;H0;D3;+0:13]2:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:2)-O-C-1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]3:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5...
85.4
[{"value": 85.4, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2CCN(CC2)C(=O)OC(C)(C)C)COCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
tert-Butyl 4-[(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)methyl]piperidine-1-carboxylate (12.79 g, 24.67 mmol) and pyrdine-3-boronic acid 1,3-propanediol cyclic ester (4.42 g, 27.14 mmol) were coupled according to the method described in Examples 118–121. The work-up procedure described in Part F of...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccc2c(c1)ncc1[nH]cnc12.B1OCCCO1.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.C1CC[NH]CC1
HBr.B
null
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7f6c6e3fc28f475d81766645384bb24d
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCNCC1.Cl.Cl
Cl.NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2CCN(CC2)C(=O)OC(C)(C)C)COCC)C=2C=NC=CC2>>Cl.Cl.Cl.C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC1CCNCC1
CC(C)(C)OC(=O)[N:29]1[CH2:28][CH2:27][CH:26]([CH2:25][n:24]2[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]3[c:8]([NH2:9])[n:10][c:11]4[cH:12][c:13](-[c:14]5[cH:15][cH:16][cH:17][n:18][cH:19]5)[cH:20][cH:21][c:22]4[c:23]32)[CH2:31][CH2:30]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCNCC1.Cl.Cl
null
null
C(C)O
Miscellaneous
Boc amine deprotection
0d17b1cd8faa9642170a265595f8fea596067098aa2d20db6ef6a923fda4571d
c95e79e18f8ea11cf22745e0eab38cab98566b1b63e7d80ee200f4cb4f94f00c
c1cncc(-c2ccc3c(c2)ncc2ncn(CC4CCNCC4)c23)c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
Ethanolic hydrochloric acid (17.68 mL of 4.25 M) was added to a solution of tert-butyl 4-{[4-amino-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-1-yl]methyl}piperidine-1-carboxylate (9.71 g, 18.8 mmol) in anhydrous ethanol, and the reaction was heated at reflux for two hours. A precipitate formed, and the r...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.C1CCNCC1
HO-
C(C)O
null
null
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1>C(C)O>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCNCC1.Cl.Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-18c55e75a5c248f0a49de337c375323e
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCNCC1.O=C(O)C1CCCO1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)C2CCCO2)CC1
Cl.Cl.Cl.C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC1CCNCC1.C(C)N(CC)CC.O1C(CCC1)C(=O)O.Cl.CON(CCCN=C=NCC)OC.ON1N=NC2=C1C=CC=C2>>C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC1CCN(CC1)C(=O)C1OCCC1
[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][cH:17][n:18][cH:19]4)[cH:20][cH:21][c:22]3[c:23]2[n:24]1[CH2:25][CH:26]1[CH2:27][CH2:28][NH:29][CH2:37][CH2:38]1.O[C:30](=[O:31])[CH:32]1[CH2:33][CH2:34][CH2:35][O:36]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCNCC1.O=C(O)C1CCCO1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)C2CCCO2)CC1
null
null
C(Cl)(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Carboxylic Acids
fbfce93ec1ece674255bb96c5cec09ad611382b41cf117dfe580015e21744a71
c5e4172490b2731ba9322b68af56376edadc31ce0bb9a3dfdea23a1817a852fd
O=C(C1CCCO1)N1CCC(Cn2cnc3cnc4cc(-c5cccnc5)ccc4c32)CC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[#8:5]-[C:6].[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]>>[C:7]-[C:8]-[N;H0;D3;+0:9](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[#8:5]-[C:6])-[C:10]-[C:11]
69.5
[{"value": 69.5, "product": "C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC1CCN(CC1)C(=O)C1OCCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
4
CELSIUS
2
HOUR
A solution of 2-ethoxymethyl-1-(piperidin-4-ylmethyl)-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine trihydrochloride (1.0 g, 1.90 mmol) and triethylamine (1.35 mL, 9.50 mmol) in chloroform (80 mL) was cooled to 4° C. 2-Tetrahydrofuroic acid (0.243 g, 2.09 mmol) and 1-(3-dimethoxyaminopropyl)-3-ethylcarbodiimide hy...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Tertiary amide
C1CCNCC1
C1CC[NH]CC1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.C1CC[NH]CC1.C1CCOC1
HO-
C(Cl)(Cl)Cl
4
2
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCNCC1.O=C(O)C1CCCO1>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)C2CCCO2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-430d0386e8414621b64afa9b24284926
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.NCCCN1C(CCC1)=O>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCN1C(CCC1)=O
[O:1]=[C:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][CH2:9][NH2:10].Cl[c:11]1[c:12]([N+:13](=[O:14])[O-:15])[cH:16][n:17][c:18]2[cH:19][c:20]([Br:21])[cH:22][cH:23][c:24]12>>[O:1]=[C:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][CH2:9][NH:10][c:11]1[c:12]([N+:13](=[O:14])[O-:15])[cH:16][n:17][c:18]2[cH:19][c:20]([Br:21...
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C1CCCN1CCCNc1ccnc2ccccc12
Cl-[c;H0;D3;+0:1]1:[c:2](-[#7;+:3]):[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8]:1:[c:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:3]-[c:2]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
84
[{"value": 84.0, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCN1C(CCC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7-Bromo-4-chloro-3-nitroquinoline (35.26 g, 123.8 mmol) was treated with 1-(3-aminopropyl)pyrrolidin-2-one (19.1 mL, 136.2 mmol) according to the method described in Part E of Example 1 to provide 40.87 g of 1-[3-(7-bromo-3-nitroquinolin-4-ylamino)propyl]pyrrolidin-2-one as a yellow solid. Conditions: See reaction.note...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
C1CC[NH]C1.c1ccc2ncccc2c1
HCl
null
null
null
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-73b5eeb65ee0473787a827af92511bab
COCCC(=O)Cl.O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>COCCc1nc2cnc3cc(Br)ccc3c2n1CCCN1CCCC1=O
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCN1C(CCC1)=O.COCCC(=O)Cl.C(C)N(CC)CC>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCN3C(CCC3)=O)CCOC
O=[C:5](Cl)[CH2:4][CH2:3][O:2][CH3:1].O=[N+:6]([O-])[c:7]1[cH:8][n:9][c:10]2[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]2[c:17]1[NH:18][CH2:19][CH2:20][CH2:21][N:22]1[CH2:23][CH2:24][CH2:25][C:26]1=[O:27]>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18...
COCCC(=O)Cl.O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
COCCc1nc2cnc3cc(Br)ccc3c2n1CCCN1CCCC1=O
null
null
null
Aromatic Heterocycle Formation
OtherReaction
f5ccfa638b9ebde84faf3ed5ae8aa34e1d73a7445584b4a71cf926baaa6ffdb4
65afb0bd4703d35942ab9e6c52b2a1e949dd1e9f7cc47623826614e8c0ed673b
O=C1CCCN1CCCn1cnc2cnc3ccccc3c21
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[C:3].O=[N+;H0;D3:4](-[O-])-[c:5]1:[c:6]:[#7;a:7]:[c:8]:[c:9]:[c:10]:1-[NH;D2;+0:11]-[C:12]-[C:13]>>[C:13]-[C:12]-[n;H0;D3;+0:11]1:[c:10]2:[c:9]:[c:8]:[#7;a:7]:[c:6]:[c:5]:2:[n;H0;D2;+0:4]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
null
[]
null
null
null
null
1-[3-(7-Bromo3-nitroquinolin-4-ylamino)propyl]pyrrolidin-2-one was treated according to the methods described in Parts B, C, and D of Examples 152–156. 3-Methoxypropionyl chloride was used in Part C, and triethylamine (1.3 equivalents) was added to the reaction mixture. The crude product obtained in Part D was purified...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Nitro group.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.C1CC[NH]C1
HCl
null
null
null
COCCC(=O)Cl.O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>COCCc1nc2cnc3cc(Br)ccc3c2n1CCCN1CCCC1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9bc5d76282ce46f99fc9bea711c2f243
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2ccc(Br)cc2c1Cl>>O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2ccc(Br)cc12
BrC=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])Cl.BrC1=CC=C(N)C=C1.NCCCN1C(CCC1)=O>>BrC=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])NCCCN1C(CCC1)=O
[O:1]=[C:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][CH2:9][NH2:10].Cl[c:11]1[c:12]([N+:13](=[O:14])[O-:15])[cH:16][n:17][c:18]2[cH:19][cH:20][c:21]([Br:22])[cH:23][c:24]12>>[O:1]=[C:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][CH2:9][NH:10][c:11]1[c:12]([N+:13](=[O:14])[O-:15])[cH:16][n:17][c:18]2[cH:19][cH:20][c:21]...
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2ccc(Br)cc2c1Cl
O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2ccc(Br)cc12
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C1CCCN1CCCNc1ccnc2ccccc12
Cl-[c;H0;D3;+0:1]1:[c:2](-[#7;+:3]):[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8]:1:[c:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:3]-[c:2]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
87.8
[{"value": 87.8, "product": "BrC=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])NCCCN1C(CCC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
6-Bromo-4-chloro-3-nitroquinoline (50.62 g, 177.8 mmol), prepared from 4-bromoaniline according to the methods described in Parts A–D of Example 1, was treated with 1-(3-aminopropyl)pyrrolidin-2-one (27.5 mL, 196 mmol) according to the method described in Part E of Example 1 to provide 61.41 g of 1-[3-(6-bromo-3-nitroq...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
C1CC[NH]C1.c1ccc2ncccc2c1
HCl
null
null
null
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2ccc(Br)cc2c1Cl>>O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2ccc(Br)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e0999a8e80fc4a5f8946b95e27730253
COCCC(=O)Cl.O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2ccc(Br)cc12>>COCCc1nc2cnc3ccc(Br)cc3c2n1CCCN1CCCC1=O
BrC=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])NCCCN1C(CCC1)=O.COCCC(=O)Cl>>BrC1=CC=2C3=C(C=NC2C=C1)N=C(N3CCCN3C(CCC3)=O)CCOC
O=[C:5](Cl)[CH2:4][CH2:3][O:2][CH3:1].O=[N+:6]([O-])[c:7]1[cH:8][n:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]2[c:17]1[NH:18][CH2:19][CH2:20][CH2:21][N:22]1[CH2:23][CH2:24][CH2:25][C:26]1=[O:27]>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]3[c:17]2[n:18...
COCCC(=O)Cl.O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2ccc(Br)cc12
COCCc1nc2cnc3ccc(Br)cc3c2n1CCCN1CCCC1=O
null
null
null
Aromatic Heterocycle Formation
OtherReaction
e5efb7579e56d5ca9ced81b81969524f7016f29e82a669fa5b2c9b856824998a
65afb0bd4703d35942ab9e6c52b2a1e949dd1e9f7cc47623826614e8c0ed673b
O=C1CCCN1CCCn1cnc2cnc3ccccc3c21
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[C:3].O=[N+;H0;D3:4](-[O-])-[c:5]1:[c:6]:[#7;a:7]:[c:8]:[c:9]:[c:10]:1-[NH;D2;+0:11]-[C:12]-[C:13]>>[C:13]-[C:12]-[n;H0;D3;+0:11]1:[c:10]2:[c:9]:[c:8]:[#7;a:7]:[c:6]:[c:5]:2:[n;H0;D2;+0:4]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
null
[]
null
null
null
null
1-[3-(6-Bromo3-nitroquinolin-4-ylamino)propyl]pyrrolidin-2-one was treated according to the methods described in Parts B, C, and D of Examples 152–156. 3-Methoxypropionyl chloride was used in Part C. The crude product obtained in Part D was recrystallized from acetonitrile. The crystals were washed with cold acetonitri...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Nitro group.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2ncc3[nH]cnc3c2c1
c1ccc2ncc3[nH]cnc3c2c1.C1CC[NH]C1
HCl
null
null
null
COCCC(=O)Cl.O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2ccc(Br)cc12>>COCCc1nc2cnc3ccc(Br)cc3c2n1CCCN1CCCC1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-49ad03b0f69c45cab1df976518211e4d
CC(C)(C)OC(=O)N1CCC(CN)CC1.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>>CC(C)(C)OC(=O)N1CCC(CNc2c([N+](=O)[O-])cnc3cc(-c4ccccc4)ccc23)CC1
ClC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-].C(C)(C)(C)OC(=O)N1CCC(CC1)CN>>[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCC1CCN(CC1)C(=O)OC(C)(C)C)C1=CC=CC=C1
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][NH2:13])[CH2:33][CH2:34]1.Cl[c:14]1[c:15]([N+:16](=[O:17])[O-:18])[cH:19][n:20][c:21]2[cH:22][c:23](-[c:24]3[cH:25][cH:26][cH:27][cH:28][cH:29]3)[cH:30][cH:31][c:32]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2...
CC(C)(C)OC(=O)N1CCC(CN)CC1.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
CC(C)(C)OC(=O)N1CCC(CNc2c([N+](=O)[O-])cnc3cc(-c4ccccc4)ccc23)CC1
null
null
C(C)OCC
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(-c2ccc3c(NCC4CCNCC4)ccnc3c2)cc1
Cl-[c;H0;D3;+0:1]1:[c:2](-[#7;+:3]):[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8]:1:[c:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:3]-[c:2]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
94.3
[{"value": 94.3, "product": "[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCC1CCN(CC1)C(=O)OC(C)(C)C)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Chloro-3-nitro-7-phenylquinoline (8.35 g, 29.3 mmol) was treated with 1-(tert-butoxycarbonyl)-4-(aminomethyl)piperidine (7.54 g, 35.2 mmol) according to the method described in Part A of Examples 152–156. The crude solid was triturated with water, isolated by filtration, sonicated with diethyl ether, isolated by filt...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
C1CC[NH]CC1.c1ccc2ncccc2c1.c1ccccc1
HCl
C(C)OCC
null
null
CC(C)(C)OC(=O)N1CCC(CN)CC1.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>C(C)OCC>CC(C)(C)OC(=O)N1CCC(CNc2c([N+](=O)[O-])cnc3cc(-c4ccccc4)ccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c56825bcfe01483a83fa38235d7cbd81
CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1>>CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC1CCNCC1
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2CCN(CC2)C(=O)OC(C)(C)C)COCC)C2=CC=CC=C2.[OH-].[NH4+]>>C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C2=CC=CC=C2)N)N1)CC1CCNCC1
CC(C)(C)OC(=O)[N:29]1[CH2:28][CH2:27][CH:26]([CH2:25][n:24]2[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]3[c:8]([NH2:9])[n:10][c:11]4[cH:12][c:13](-[c:14]5[cH:15][cH:16][cH:17][cH:18][cH:19]5)[cH:20][cH:21][c:22]4[c:23]32)[CH2:31][CH2:30]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:1...
CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC1CCNCC1
null
null
O
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc(-c2ccc3c(c2)ncc2ncn(CC4CCNCC4)c23)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
54.3
[{"value": 54.3, "product": "C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C2=CC=CC=C2)N)N1)CC1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
tert-Butyl 4-[(4-amino-2-ethoxymethyl-7-phenyl-1H-imidazo[4,5-c]quinolin-1-yl)methyl]piperidine-1-carboxylate (0.64 g) was deprotected according to the method described in Example 177. The crude solid was dissolved in water (10 mL), and ammonium hydroxide was added until the solution was basic. The mixture was then ext...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1.C1CCNCC1
HO-
O
null
null
CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1>O>CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CC1CCNCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f72f99ec1a3a4a8dbe5376dce345964e
NCCOc1ccccc1.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>>O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1
ClC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-].O(C1=CC=CC=C1)CCN>>[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCCOC1=CC=CC=C1)C1=CC=CC=C1
[NH2:20][CH2:21][CH2:22][O:23][c:24]1[cH:25][cH:26][cH:27][cH:28][cH:29]1.Cl[c:19]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][c:9](-[c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[cH:16][cH:17][c:18]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][c:9](-[c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[cH:16][cH:1...
NCCOc1ccccc1.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1
null
null
C(C)OCC
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(OCCNc2ccnc3cc(-c4ccccc4)ccc23)cc1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
100.3
[{"value": 100.3, "product": "[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCCOC1=CC=CC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Chloro-3-nitro-7-phenylquinoline (6.0 g, 21 mmol) was treated with 2-phenoxyethylamine (3.18 g, 23.2 mmol) according to the method described in Part A of Examples 125–135. The crude solid was triturated with water (100 mL), isolated by filtration, sonicated with diethyl ether, isolated by filtration, and dried for tw...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1.c1ccccc1
HCl
C(C)OCC
null
null
NCCOc1ccccc1.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>C(C)OCC>O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c6f8ff1a6e6447ae9d0992d40f4400f0
O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1>>Nc1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1
[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCCOC1=CC=CC=C1)C1=CC=CC=C1>>O(C1=CC=CC=C1)CCNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)N
O=[N+:1]([O-])[c:2]1[cH:3][n:4][c:5]2[cH:6][c:7](-[c:8]3[cH:9][cH:10][cH:11][cH:12][cH:13]3)[cH:14][cH:15][c:16]2[c:17]1[NH:18][CH2:19][CH2:20][O:21][c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1>>[NH2:1][c:2]1[cH:3][n:4][c:5]2[cH:6][c:7](-[c:8]3[cH:9][cH:10][cH:11][cH:12][cH:13]3)[cH:14][cH:15][c:16]2[c:17]1[NH:18][CH2:1...
O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1
Nc1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1
null
[Pt]
CO
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(OCCNc2ccnc3cc(-c4ccccc4)ccc23)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
null
[]
null
null
null
null
A solution of (3-nitro-7-phenylquinolin-4-yl)-(2-phenoxyethyl)amine (7.25 g, 18.8 mmol) in methanol (150 mL) was added to a Parr vessel charged with 5% platinum on carbon (0.84 g), and the reaction was placed under hydrogen pressure (50 psi, 3.4×105 Pa) for three hours. The reaction mixture was filtered through a layer...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1.c1ccccc1.c1ccccc1
Other
[Pt].CO
null
null
O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1>[Pt].CO>Nc1cnc2cc(-c3ccccc3)ccc2c1NCCOc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6adf18b19dfd401ca036b2c8938a2b96
CC(C)(C)OC(=O)NCCCCN.CS(=O)(=O)Cl>>CC(C)(C)OC(=O)NCCCCNS(C)(=O)=O
NCCCCNC(OC(C)(C)C)=O.C(C)N(CC)CC.CS(=O)(=O)Cl>>CS(=O)(=O)NCCCCNC(OC(C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][CH2:12][NH2:13].Cl[S:14]([CH3:15])(=[O:16])=[O:17]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:13][S:14]([CH3:15])(=[O:16])=[O:17]
CC(C)(C)OC(=O)NCCCCN.CS(=O)(=O)Cl
CC(C)(C)OC(=O)NCCCCNS(C)(=O)=O
null
null
C(C)(=O)O
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
null
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:5]-[C:6]-[NH;D2;+0:7]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
96.7
[{"value": 96.7, "product": "CS(=O)(=O)NCCCCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Under a nitrogen atmosphere, a solution of tert-butyl N-(4-aminobutyl)carbamate (13.8 g, 73.4 mmol) and triethylamine (15.3 mL, 110 mmol) was cooled to 0° C. Methanesulfonyl chloride (6.3 mL, 81 mmol) was added, and the reaction was allowed to warm to ambient temperature and stirred overnight. Aqueous acetic acid (200 ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
null
HCl
C(C)(=O)O
null
8
CC(C)(C)OC(=O)NCCCCN.CS(=O)(=O)Cl>C(C)(=O)O>CC(C)(C)OC(=O)NCCCCNS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3e1f5abfa6d942d1a82cf7baca23135b
CC(C)(C)OC(=O)NCCCCNS(C)(=O)=O>>CS(=O)(=O)NCCCCN
Cl.CS(=O)(=O)NCCCCNC(OC(C)(C)C)=O>>Cl.NCCCCNS(=O)(=O)C
CC(C)(C)OC(=O)[NH:10][CH2:9][CH2:8][CH2:7][CH2:6][NH:5][S:2]([CH3:1])(=[O:3])=[O:4]>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][CH2:6][CH2:7][CH2:8][CH2:9][NH2:10]
CC(C)(C)OC(=O)NCCCCNS(C)(=O)=O
CS(=O)(=O)NCCCCN
null
null
C(C)O
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
null
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
100
CELSIUS
null
null
A solution of hydrochloric acid in ethanol was added to a solution of tert-butyl [4-(methanesulfonylamino)butyl]carbamate (18.9 g, 71.1 mmol) in ethanol (100 mL), and the reaction was heated at 100° C. for two hours. The solvent was removed under reduced pressure. A mixture of dichloromethane:hexanes was added to the r...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
null
HO-
C(C)O
100
null
CC(C)(C)OC(=O)NCCCCNS(C)(=O)=O>C(C)O>CS(=O)(=O)NCCCCN
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8fccf99693c64fad9f96b1c8c8faeb9d
CS(=O)(=O)NCCCCN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>>CS(=O)(=O)NCCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
O.Cl.NCCCCNS(=O)(=O)C.ClC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-].C(C)N(CC)CC>>[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCCCCNS(=O)(=O)C)C1=CC=CC=C1
[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][CH2:6][CH2:7][CH2:8][CH2:9][NH2:10].Cl[c:11]1[c:12]([N+:13](=[O:14])[O-:15])[cH:16][n:17][c:18]2[cH:19][c:20](-[c:21]3[cH:22][cH:23][cH:24][cH:25][cH:26]3)[cH:27][cH:28][c:29]12>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][CH2:6][CH2:7][CH2:8][CH2:9][NH:10][c:11]1[c:12]([N+:13](=[O:14])[O-:15]...
CS(=O)(=O)NCCCCN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
CS(=O)(=O)NCCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
null
null
CN1CCCC1=O
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(-c2ccc3cccnc3c2)cc1
Cl-[c;H0;D3;+0:1]1:[c:2](-[#7;+:3]):[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8]:1:[c:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:3]-[c:2]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
82.7
[{"value": 82.7, "product": "[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCCCCNS(=O)(=O)C)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
N-(4-aminobutyl)methanesulfonamide hydrochloride (7.8 g, 39 mmol) was added to a suspension of 4-chloro-3-nitro-7-phenylquinoline (35 mmol) and triethylamine (8.0 g, 79 mmol) in NMP (80 mL), and the reaction was stirred at ambient temperature overnight. The resulting solution was poured into water (350 mL) to form a so...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HCl
CN1CCCC1=O
null
8
CS(=O)(=O)NCCCCN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>CN1CCCC1=O>CS(=O)(=O)NCCCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-488bb10254d64e94955ce5a59e9d54b2
CC(C)(N)CN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>>CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
ClC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-].NCC(C)(C)N.C(C)N(CC)CC>>[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCC(C)(N)C)C1=CC=CC=C1
[CH3:1][C:2]([CH3:3])([NH2:4])[CH2:5][NH2:6].Cl[c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16](-[c:17]3[cH:18][cH:19][cH:20][cH:21][cH:22]3)[cH:23][cH:24][c:25]12>>[CH3:1][C:2]([CH3:3])([NH2:4])[CH2:5][NH:6][c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16](-[c:17]3[cH:18][cH:19][...
CC(C)(N)CN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
null
null
ClCCl
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(-c2ccc3cccnc3c2)cc1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
null
[]
null
null
null
null
A solution of 1,2-diamino-2-methylpropane (9.3 mL, 88.9 mmol) and triethylamine (5.0 mL, 35.5 mmol) in dichloromethane (100 mL) was cooled to 0° C. A solution of 4-chloro-3-nitro-7-phenylquinoline (5.06 g, 17.8 mmol) in dichloromethane (50 mL) was added over a period of 45 minutes, and then the reaction was allowed to ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1
HCl
ClCCl
null
null
CC(C)(N)CN.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>ClCCl>CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b1f64bdf6e76463192b17da361ab9967
CC(C)(CNc1c(N)cnc2cc(-c3ccccc3)ccc12)NS(C)(=O)=O.CCCC(OC)(OC)OC>>CCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CC(C)(C)NS(C)(=O)=O
NC=1C=NC2=CC(=CC=C2C1NCC(C)(C)NS(=O)(=O)C)C1=CC=CC=C1.C(CCC)(OC)(OC)OC>>C1(=CC=CC=C1)C=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(C)NS(=O)(=O)C)CCC
[NH2:5][c:6]1[cH:7][n:8][c:9]2[cH:10][c:11](-[c:12]3[cH:13][cH:14][cH:15][cH:16][cH:17]3)[cH:18][cH:19][c:20]2[c:21]1[NH:22][CH2:23][C:24]([CH3:25])([CH3:26])[NH:27][S:28]([CH3:29])(=[O:30])=[O:31].CO[C:4](OC)(OC)[CH2:3][CH2:2][CH3:1]>>[CH3:1][CH2:2][CH2:3][c:4]1[n:5][c:6]2[cH:7][n:8][c:9]3[cH:10][c:11](-[c:12]4[cH:13]...
CC(C)(CNc1c(N)cnc2cc(-c3ccccc3)ccc12)NS(C)(=O)=O.CCCC(OC)(OC)OC
CCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CC(C)(C)NS(C)(=O)=O
null
null
null
Aromatic Heterocycle Formation
OtherReaction
8d87c769e65778c9400c7f523e0409ecf0ffad86543cd9fdd6ef4b239323db96
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc(-c2ccc3c(c2)ncc2nc[nH]c23)cc1
C-O-[C;H0;D4;+0:1](-O-C)(-O-C)-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
81.8
[{"value": 81.8, "product": "C1(=CC=CC=C1)C=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(C)NS(=O)(=O)C)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
N-[2-(3-Amino-7-phenylquinolin-4-ylamino)-1,1-dimethylethyl]methanesulfonamide (2.20 g, 5.04 mmol) was treated with trimethyl orthobutyrate (0.90 mL, 5.5 mmol) according to the method described in Part G of Example 1. The chromatographic purification was carried out eluting with 92.5:7.5 dichloromethane:methanol to pro...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HO-
null
null
null
CC(C)(CNc1c(N)cnc2cc(-c3ccccc3)ccc12)NS(C)(=O)=O.CCCC(OC)(OC)OC>>CCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CC(C)(C)NS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f15ea28ffbee4c82a8f9b5a3dcec7661
CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12.O=C(Cl)C1CCCCC1>>C1CCCCC1.CC(C)(CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12)NC=O
[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCC(C)(N)C)C1=CC=CC=C1.C(C)N(CC)CC.C1(CCCCC1)C(=O)Cl>>CC(CNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-])(C)NC=O.C1CCCCC1
[CH3:7][C:8]([CH3:9])([CH2:10][NH:11][c:12]1[c:13]([N+:14](=[O:15])[O-:16])[cH:17][n:18][c:19]2[cH:20][c:21](-[c:22]3[cH:23][cH:24][cH:25][cH:26][cH:27]3)[cH:28][cH:29][c:30]12)[NH2:31].Cl[C:32]([CH:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1)=[O:33]>>[CH2:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1.[CH3:7][C:8]([CH3:9])([CH2:...
CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12.O=C(Cl)C1CCCCC1
C1CCCCC1.CC(C)(CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12)NC=O
null
null
ClCCl
Acylation
OtherReaction
8d2371177cf46fb9dc57ec883e4d22ded454c0442f6ab5d8c6007193fa4dba33
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
C1CCCCC1.c1ccc(-c2ccc3cccnc3c2)cc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH;D3;+0:3](-[C:4]-[C:5])-[C:6]-[C:7].[C:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[NH2;D1;+0:12]>>[C:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[NH;D2;+0:12]-[CH;D2;+0:1]=[O;D1;H0:2].[C:5]-[C:4]-[CH2;D2;+0:3]-[C:6]-[C:7]
70
[{"value": 70.0, "product": "CC(CNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-])(C)NC=O.C1CCCCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A solution of N1-(3-nitro-7-phenylquinolin-4-yl)-2-methylpropane-1,2-diamine (3.56 g, 10.6 mmol) in dichloromethane (100 mL) was cooled to 0° C. Triethylamine (3.0 mL, 21 mmol) and cyclohexanecarbonyl chloride (1.55 mL, 11.6 mmol) were sequentially added. The reaction was allowed to warm to ambient temperature and stir...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
C1CCCCC1
C1CCCCC1
C1CCCCC1.c1ccc2ncccc2c1.c1ccccc1
Other
ClCCl
null
2
CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12.O=C(Cl)C1CCCCC1>ClCCl>C1CCCCC1.CC(C)(CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12)NC=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9d81f920428647a890f47a570c783a86
CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12.O=C=NC1CCCCC1>>CC(C)(CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12)NC(=O)NC1CCCCC1
[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCC(C)(N)C)C1=CC=CC=C1.C1(CCCCC1)N=C=O>>C1(CCCCC1)NC(=O)NC(CNC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-])(C)C
[CH3:1][C:2]([CH3:3])([CH2:4][NH:5][c:6]1[c:7]([N+:8](=[O:9])[O-:10])[cH:11][n:12][c:13]2[cH:14][c:15](-[c:16]3[cH:17][cH:18][cH:19][cH:20][cH:21]3)[cH:22][cH:23][c:24]12)[NH2:25].[C:26](=[O:27])=[N:28][CH:29]1[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34]1>>[CH3:1][C:2]([CH3:3])([CH2:4][NH:5][c:6]1[c:7]([N+:8](=[O:9])[O-:10...
CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12.O=C=NC1CCCCC1
CC(C)(CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12)NC(=O)NC1CCCCC1
null
null
ClCCl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
O=C(NCCNc1ccnc2cc(-c3ccccc3)ccc12)NC1CCCCC1
[C:1]-[C:2](-[C;D1;H3:3])(-[C;D1;H3:4])-[NH2;D1;+0:5].[C:6]-[C:7](-[N;H0;D2;+0:8]=[C;H0;D2;+0:9]=[O;D1;H0:10])-[C:11]>>[C:6]-[C:7](-[NH;D2;+0:8]-[C;H0;D3;+0:9](=[O;D1;H0:10])-[NH;D2;+0:5]-[C:2](-[C:1])(-[C;D1;H3:3])-[C;D1;H3:4])-[C:11]
null
[]
null
null
3
DAY
A solution of N1-(3-nitro-7-phenylquinolin-4-yl)-2-methylpropane-1,2-diamine (3.56 g, 10.6 mmol) in dichloromethane (100 mL) was cooled to 0° C. Cyclohexyl isocyanate (3.00 mL, 23.5 mmol) was added over the course of a day, and the reaction was stirred at ambient temperature for three days. The solvent was removed unde...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccc2ncccc2c1.c1ccccc1.C1CCCCC1
null
ClCCl
null
72
CC(C)(N)CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12.O=C=NC1CCCCC1>ClCCl>CC(C)(CNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12)NC(=O)NC1CCCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f0308dc5638740e99da368b42ceb3de7
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>>O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
ClC1=C(C=NC2=CC(=CC=C12)C1=CC=CC=C1)[N+](=O)[O-].NCCCN1C(CCC1)=O>>[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCCCN1C(CCC1)=O)C1=CC=CC=C1
[O:1]=[C:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][CH2:9][NH2:10].Cl[c:11]1[c:12]([N+:13](=[O:14])[O-:15])[cH:16][n:17][c:18]2[cH:19][c:20](-[c:21]3[cH:22][cH:23][cH:24][cH:25][cH:26]3)[cH:27][cH:28][c:29]12>>[O:1]=[C:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][CH2:9][NH:10][c:11]1[c:12]([N+:13](=[O:14])[O-:15])[cH...
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl
O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C1CCCN1CCCNc1ccnc2cc(-c3ccccc3)ccc12
Cl-[c;H0;D3;+0:1]1:[c:2](-[#7;+:3]):[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8]:1:[c:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:3]-[c:2]1:[c:4]:[#7;a:5]:[c:6](:[c:7]):[c:8](:[c:9]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
88.1
[{"value": 88.1, "product": "[N+](=O)([O-])C=1C=NC2=CC(=CC=C2C1NCCCN1C(CCC1)=O)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Chloro-3-nitro-7-phenylquinoline (3.51 g, 12.3 mmol) was treated with 1-(3-aminopropyl)pyrrolidin-2-one (2.3 mL, 16 mmol) according to the method described in Part E of Example 1 to provide 4.23 g of 1-[3-(3-nitro-7-phenylquinolin-4-ylamino)propyl]pyrrolidin-2-one as a yellow solid. Conditions: See reaction.notes.pro...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
C1CC[NH]C1.c1ccc2ncccc2c1.c1ccccc1
HCl
null
null
null
NCCCN1CCCC1=O.O=[N+]([O-])c1cnc2cc(-c3ccccc3)ccc2c1Cl>>O=C1CCCN1CCCNc1c([N+](=O)[O-])cnc2cc(-c3ccccc3)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f18f803e88054fb58ebacb523833a126
CCOCC(=O)Cl.Nc1cnc2cc(-c3ccccc3)ccc2c1NCCCN1CCCC1=O>>CCOCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCN1CCCC1=O
NC=1C=NC2=CC(=CC=C2C1NCCCN1C(CCC1)=O)C1=CC=CC=C1.C(C)OCC(=O)Cl.C(C)N(CC)CC>>C(C)OCC=1N(C2=C(C=NC=3C=C(C=CC23)C2=CC=CC=C2)N1)CCCN1C(CCC1)=O
O=[C:5](Cl)[CH2:4][O:3][CH2:2][CH3:1].[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][c:12](-[c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)[cH:19][cH:20][c:21]2[c:22]1[NH:23][CH2:24][CH2:25][CH2:26][N:27]1[CH2:28][CH2:29][CH2:30][C:31]1=[O:32]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12](-[c:13]4[cH...
CCOCC(=O)Cl.Nc1cnc2cc(-c3ccccc3)ccc2c1NCCCN1CCCC1=O
CCOCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCN1CCCC1=O
null
null
null
Aromatic Heterocycle Formation
OtherReaction
101a087a520f159c722ba3d78ed38f5c3c1cf154206e5edbeb1e6397c929560f
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
O=C1CCCN1CCCn1cnc2cnc3cc(-c4ccccc4)ccc3c21
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[#8:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[#8:3]-[C:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:13]:[c:12]2:[c:11]:[#7;a:10]:[c:9]:[c:8]:[c:7]:2:[n;H0;D3;+0:6]:1-[C:5]-[C:4]
56.7
[{"value": 56.7, "product": "C(C)OCC=1N(C2=C(C=NC=3C=C(C=CC23)C2=CC=CC=C2)N1)CCCN1C(CCC1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
1-[3-(3-Amino-7-phenylquinolin-4-ylamino)propyl]pyrrolidin-2-one (2.21 g, 6.13 mmol) was treated with ethoxyacetyl chloride (0.95 mL, 8.76 mmol) according to the methods described in Parts C and D of Examples 152–156. Triethylamine (8.6 mmol) was added in Part C. The product from Part D was purified by column chromatog...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1.C1CC[NH]C1
HCl
null
null
null
CCOCC(=O)Cl.Nc1cnc2cc(-c3ccccc3)ccc2c1NCCCN1CCCC1=O>>CCOCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCN1CCCC1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-26d6796ecf234855b1356d51dc24084a
COCCC(=O)Cl.Nc1cnc2cc(-c3ccccc3)ccc2c1NCCCN1CCCC1=O>>COCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCN1CCCC1=O
NC=1C=NC2=CC(=CC=C2C1NCCCN1C(CCC1)=O)C1=CC=CC=C1.COCCC(=O)Cl>>COCCC=1N(C2=C(C=NC=3C=C(C=CC23)C2=CC=CC=C2)N1)CCCN1C(CCC1)=O
O=[C:5](Cl)[CH2:4][CH2:3][O:2][CH3:1].[NH2:6][c:7]1[cH:8][n:9][c:10]2[cH:11][c:12](-[c:13]3[cH:14][cH:15][cH:16][cH:17][cH:18]3)[cH:19][cH:20][c:21]2[c:22]1[NH:23][CH2:24][CH2:25][CH2:26][N:27]1[CH2:28][CH2:29][CH2:30][C:31]1=[O:32]>>[CH3:1][O:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12](-[c:13]4[cH...
COCCC(=O)Cl.Nc1cnc2cc(-c3ccccc3)ccc2c1NCCCN1CCCC1=O
COCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCN1CCCC1=O
null
null
null
Aromatic Heterocycle Formation
OtherReaction
101a087a520f159c722ba3d78ed38f5c3c1cf154206e5edbeb1e6397c929560f
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
O=C1CCCN1CCCn1cnc2cnc3cc(-c4ccccc4)ccc3c21
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[C:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C:3]
null
[]
null
null
null
null
The methods described in Parts A of Example 204 were used to treat 1-[3-(3-amino-7-phenylquinolin-4-ylamino)propyl]pyrrolidin-2-one (1.19 g, 3.30 mmol) with 3-methoxypropionyl chloride (0.45 mL, 4.1 mmol) to afford 1-{3-[2-(2-methoxyethyl)-7-phenyl-1H-imidazo[4,5-c]quinolin-1-yl]propyl}pyrrolidin-2-one, which was oxidi...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1.C1CC[NH]C1
HCl
null
null
null
COCCC(=O)Cl.Nc1cnc2cc(-c3ccccc3)ccc2c1NCCCN1CCCC1=O>>COCCc1nc2cnc3cc(-c4ccccc4)ccc3c2n1CCCN1CCCC1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4e57e73174c846a0ad0b36fef32f9e8b
C=CS(C)(=O)=O.CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O
O.C(=C)S(=O)(=O)C.BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)COCC.[H-].[Na+]>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(C)OCCS(=O)(=O)C)COCC
[CH2:24]=[CH:25][S:26]([CH3:27])(=[O:28])=[O:29].[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][C:20]([CH3:21])([CH3:22])[OH:23]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]...
C=CS(C)(=O)=O.CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
oxa-Michael addition
714eaa0e6de1d85d58a88133b4d5e95857344ec278e90cde0496674a55b79739
ea8641c928da9fe5f2bca5bb859dbb223e9e99eefdf70a15450fd2e768112e0a
c1ccc2c(c1)ncc1nc[nH]c12
[C;D1;H3:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[CH;D2;+0:5]=[CH2;D1;+0:6].[C:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[OH;D1;+0:11]>>[C:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[O;H0;D2;+0:11]-[CH2;D2;+0:6]-[CH2;D2;+0:5]-[#16:2](-[C;D1;H3:1])(=[O;D1;H0:3])=[O;D1;H0:4]
null
[]
null
null
70
MINUTE
A solution of methyl vinyl sulfone (3.0 g, 29 mmol) and 1-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)-2-methylpropan-2-ol (5.4 g, 14 mmol) in anhydrous THF (57 mL) was purged with nitrogen; solid sodium hydride (available as a 60% dispersion in mineral oil, 57 mg, 1.4 mmol) was added. The reaction was stirr...
10.6084/m9.figshare.5104873.v1
null
Tertiary alcohol.Vinyl
Ether
null
null
c1ccc2c(c1)ncc1[nH]cnc12
null
C1CCOC1
null
1.166667
C=CS(C)(=O)=O.CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O>C1CCOC1>CCOCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4e9c85fdd7b549379978a18932e2d098
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)(C)OCCS(=O)(=O)C)COCC.B1(OCCCO1)C2=CN=CC=C2>>C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC(C)(C)OCCS(=O)(=O)C
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:24]([CH2:25][C:26]([CH3:27])([CH3:28])[O:29][CH2:30][CH2:31][S:32]([CH3:33])(=[O:34])=[O:35])[c:23]3[c:22]2[cH:21][cH:20]1.C1COB([c:14]2[cH:15][cH:16][cH:17][n:18][cH:19]2)OC1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O.c1cncc(B2OCCCO2)c1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O
null
null
null
C-C Coupling
Suzuki coupling with boronic esters
2cd1cbe6f17c98cb5223a75d20dfc144a6eae8461c4fe8a7e9cc4bc7ecadb166
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.C1-C-O-B(-[c;H0;D3;+0:13]2:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:2)-O-C-1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]3:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5...
58.6
[{"value": 58.6, "product": "C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC(C)(C)OCCS(=O)(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7-Bromo-2-ethoxymethyl-1-{2-[2-(methanesulfonyl)ethoxy]-2-methylpropyl}-1H-imidazo[4,5-c]quinolin-4-amine (1.2 g, 2.4 mmol) and pyridine-3-boronic acid 1,3-propanediol cyclic ester (0.47 g, 2.9 mmol) were coupled according to the method described in Part J of Example 1. The work-up procedure used in Part F of Examples ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccc2c(c1)ncc1[nH]cnc12.B1OCCCO1.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HBr.B
null
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC(C)(C)OCCS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-27596081b9574913b377010ca438e260
NCCCCO.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCO
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.NCCCCO.NCCCCO>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCCO
[NH2:15][CH2:16][CH2:17][CH2:18][CH2:19][OH:20].Cl[c:14]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]2[c:14]1[NH:15][CH2:16][CH2:17][CH2:18][CH2:19][OH:20]
NCCCCO.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCO
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2ncccc2c1
Cl-[c;H0;D3;+0:1]1:[c:2](:[c:3]):[c:4](:[c:5]):[#7;a:6]:[c:7]:[c:8]:1-[#7;+:9].[C:10]-[C:11]-[NH2;D1;+0:12]>>[#7;+:9]-[c:8]1:[c:7]:[#7;a:6]:[c:4](:[c:5]):[c:2](:[c:3]):[c;H0;D3;+0:1]:1-[NH;D2;+0:12]-[C:11]-[C:10]
89.1
[{"value": 89.1, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A modification of the method described in Part E of Example 1 was used to treat 7-bromo-4-chloro-3-nitroquinoline (20.0 g, 69.6 mmol) with 4-amino-1-butanol (6.9 mL, 76.5 mmol). The addition of 4-amino-1-butanol was carried out at ambient temperature. The product, 4-(7-bromo-3-nitroquinolin-4-ylamino)butan-1-ol (21.1 g...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
null
null
null
NCCCCO.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCO
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b222e38a54a5496bb7a0423bbddccd3a
O=S(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCO>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCl
S(=O)(Cl)Cl.S(=O)(Cl)Cl.BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCCO.C([O-])(O)=O.[Na+]>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCCCl
O=S(Cl)[Cl:20].O[CH2:19][CH2:18][CH2:17][CH2:16][NH:15][c:14]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]2[c:14]1[NH:15][CH2:16][CH2:17][CH2:18][CH2:19][Cl:20]
O=S(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCO
O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCl
null
null
ClCCl
Functional Group Interconversion
Alcohol to chloride_SOCl2
bb752b9027dc4488ba075e5955118a819f80cabd751a7497b67c2eeb1db6b071
cbf41c7cf9fe6b47a243b1674d74ed5bf46a151f7f3a71d206e23176e158facf
c1ccc2ncccc2c1
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3]-[C:4]>>[C:4]-[C:3]-[CH2;D2;+0:2]-[Cl;H0;D1;+0:1]
37.9
[{"value": 37.9, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCCCl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
5
MINUTE
A suspension of 4-(7-bromo-3-nitroquinolin-4-ylamino)butan-1-ol (20.75 g, 61.0 mmol) in dichloromethane (220 mL) was cooled to 0° C.; thionyl chloride (4.90 mL, 67.1 mmol) was added dropwise over a period of ten minutes. The reaction was stirred at 0° C. for five minutes, allowed to warm to ambient temperature, and sti...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Primary halide
null
null
c1ccc2ncccc2c1
HCl
ClCCl
0
0.083333
O=S(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCO>ClCCl>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-440122c60b11499ca2604e0ffa81145b
O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCl>>Nc1cnc2cc(Br)ccc2c1NCCCCCl
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCCCl.S(=O)([O-])S(=O)[O-].[Na+].[Na+]>>BrC1=CC=C2C(=C(C=NC2=C1)N)NCCCCCl
O=[N+:1]([O-])[c:2]1[cH:3][n:4][c:5]2[cH:6][c:7]([Br:8])[cH:9][cH:10][c:11]2[c:12]1[NH:13][CH2:14][CH2:15][CH2:16][CH2:17][Cl:18]>>[NH2:1][c:2]1[cH:3][n:4][c:5]2[cH:6][c:7]([Br:8])[cH:9][cH:10][c:11]2[c:12]1[NH:13][CH2:14][CH2:15][CH2:16][CH2:17][Cl:18]
O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCl
Nc1cnc2cc(Br)ccc2c1NCCCCCl
null
null
CO.O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2ncccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
98
[{"value": 98.0, "product": "BrC1=CC=C2C(=C(C=NC2=C1)N)NCCCCCl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
A suspension of (7-bromo-3-nitroquinolin-4-yl)-(4-chlorobutyl)amine (8.05 g, 22.5 mmol) in methanol (250 mL) was cooled to 0° C.; a solution of sodium hydrosulfite (19.5 g, 112 mmol) in water (80 mL) was added dropwise over a period of 30 minutes. The reaction was stirred at ambient temperature for two hours and then c...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
CO.O
0
2
O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCl>CO.O>Nc1cnc2cc(Br)ccc2c1NCCCCCl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5addcc65777f49a1b27a679dec305ec4
CCOCC(=O)Cl.Nc1cnc2cc(Br)ccc2c1NCCCCCl>>CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCCCCCl.Cl
BrC1=CC=C2C(=C(C=NC2=C1)N)NCCCCCl.C(C)OCC(=O)Cl>>Cl.BrC1=CC=C2C(=C(C=NC2=C1)NC(COCC)=O)NCCCCCl
[CH3:1][CH2:2][O:3][CH2:4][C:5](=[O:6])[Cl:25].[NH2:7][c:8]1[cH:9][n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[c:18]1[NH:19][CH2:20][CH2:21][CH2:22][CH2:23][Cl:24]>>[CH3:1][CH2:2][O:3][CH2:4][C:5](=[O:6])[NH:7][c:8]1[cH:9][n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[c:18]1[NH:19][CH2:20][CH2:21]...
CCOCC(=O)Cl.Nc1cnc2cc(Br)ccc2c1NCCCCCl
CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCCCCCl.Cl
null
null
null
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccc2ncccc2c1
[#8:1]-[C:2]-[C;H0;D3;+0:3](-[Cl;H0;D1;+0:4])=[O;D1;H0:5].[NH2;D1;+0:6]-[c:7](:[c:8]):[c:9]:[#7;a:10]:[c:11]>>[#8:1]-[C:2]-[C;H0;D3;+0:3](=[O;D1;H0:5])-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]:[#7;a:10]:[c:11].[ClH;D0;+0:4]
null
[]
null
null
1
HOUR
A modification of the method described in Part C of Examples 125–135 was used to treat 7-bromo-N4-(4-chlorobutyl)quinoline-3,4-diamine (7.25 g, 22.1 mmol) with ethoxyacetyl chloride (2.76 mL, 24.3 mmol). After the reaction was stirred for one hour, it was concentrated under reduced pressure to provide N-[7-bromo-4-(4-c...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2ncccc2c1
null
null
null
1
CCOCC(=O)Cl.Nc1cnc2cc(Br)ccc2c1NCCCCCl>>CCOCC(=O)Nc1cnc2cc(Br)ccc2c1NCCCCCl.Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b29e7842b37f4e659459e8c871f8b783
CC([O-])=S.CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCl>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCSC(C)=O
C(C)(=S)[O-].[K+].BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCCl)COCC>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCSC(C)=O)COCC
[S:23]=[C:24]([CH3:25])[O-:26].Cl[CH2:22][CH2:21][CH2:20][CH2:19][n:18]1[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]21>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20...
CC([O-])=S.CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCl
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCSC(C)=O
null
null
CN(C)C=O
Acylation
OtherReaction
1f876542c8a2de0f0c93c1e55257e1922650fd69ea48617e41a961445109d4b2
00ab4047825d93b84a3dc255ab210414ba88fbe19a5ef7a3657605acca13230b
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[CH2;D2;+0:1]-[C:2]-[C:3].[C;D1;H3:4]-[C;H0;D3;+0:5](-[O-;H0;D1:6])=[S;H0;D1;+0:7]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:7]-[C;H0;D3;+0:5](-[C;D1;H3:4])=[O;H0;D1;+0:6]
103.4
[{"value": 103.4, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCSC(C)=O)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
21
HOUR
Potassium thioacetate (1.70 g, 14.9 mmol) was added in one portion to a stirred solution of 7-bromo-1-(4-chlorobutyl)-2-ethoxymethyl-1H-imidazo[4,5-c]quinoline (5.37 g, 13.5 mmol) in DMF (65 mL), and the reaction was stirred at ambient temperature for 21 hours. The DMF was removed under reduced pressure, and the residu...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiocarbonyl
Carbo-thioester
null
null
c1ccc2c(c1)ncc1[nH]cnc12
Other
CN(C)C=O
null
21
CC([O-])=S.CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCl>CN(C)C=O>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCSC(C)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-01d1ddd9c69b40269354404d79ae9fd0
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCSC(C)=O>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCS
BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCSC(C)=O)COCC.C[O-].[Na+]>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCS)COCC
CC(=O)[S:23][CH2:22][CH2:21][CH2:20][CH2:19][n:18]1[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]21>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][CH2:21][CH2:22][SH:...
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCSC(C)=O
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCS
null
null
CO
Reduction
OtherReaction
7702cd666d5d9a9f1bdea3600e3b84cc62dd11d3f2cea261702317a39db4e581
18d802456fe85193570fdb3a00b25c8956a03b5a0210f708f961e42c1669d76e
c1ccc2c(c1)ncc1nc[nH]c12
C-C(=O)-[S;H0;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[SH;D1;+0:1]
99.3
[{"value": 99.3, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCS)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
Nitrogen was bubbled through a solution of thioacetic acid S-[4-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)butyl]ester (1.93 g, 4.42 mmol) in methanol (45 mL), and then sodium methoxide (2.5 mL of 25% by weight in methanol, 11.1 mmol) was added dropwise over a period of three minutes. The yellow solution wa...
10.6084/m9.figshare.5104873.v1
null
Carbo-thioester
Aliphatic thiol
null
null
c1ccc2c(c1)ncc1[nH]cnc12
HO-
CO
null
1
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCSC(C)=O>CO>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCS
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-83171146c9b84b97aff0b1aa7d924e60
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O.[NH4+]>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O
ClC=1C=C(C(=O)OO)C=CC1.CC(CCCN1C(=NC=2C=NC=3C=C(C=CC3C21)Br)COCC)(S(=O)(=O)N)C.[OH-].[NH4+].C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>CC(CCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)(S(=O)(=O)N)C
[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:10][c:11]3[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]3[c:18]2[n:19]1[CH2:20][CH2:21][CH2:22][C:23]([CH3:24])([CH3:25])[S:26]([NH2:27])(=[O:28])=[O:29].[NH4+:9]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13]([Br:14])[cH:15][cH:16][c...
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O.[NH4+]
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O
null
null
ClCCl.C(Cl)(Cl)Cl
Functional Group Addition
OtherReaction
dc63235befaaf41df35292b6862b726098d8e1b79a2cef881f35b7cf9ff16606
d69ce1fde4173969963123914389bef807fad83b73b8a587195a7122d5cdf1d2
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[cH;D2;+0:6]:[#7;a:7]:[c:8]:[c:9]:[c:10]:1:2.[NH4+;D0:11]>>[C:1]-[#7;a:2]1:[c:3]:[#7;a:4]:[c:5]2:[c:10]:1:[c:9]:[c:8]:[#7;a:7]:[c;H0;D3;+0:6]:2-[NH2;D1;+0:11]
null
[]
null
null
2
HOUR
3-Chloroperoxybenzoic acid (0.126 g of 70% pure material, 0.73 mmol) was added in one portion to a stirred solution of dimethyl 4-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)butane-1-sulfonamide (0.30 g, 0.63 mmol) in chloroform (7 mL), and the solution was stirred for two hours at ambient temperature. Ammon...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
null
ClCCl.C(Cl)(Cl)Cl
null
2
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O.[NH4+]>ClCCl.C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a616420e3c0545a6852c5145c960a6c0
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O.OB(O)c1ccccc1>>CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CCCC(C)(C)S(N)(=O)=O
CC(CCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)(S(=O)(=O)N)C.C1(=CC=CC=C1)B(O)O>>CC(CCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C2=CC=CC=C2)N)COCC)(S(=O)(=O)N)C
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:24]([CH2:25][CH2:26][CH2:27][C:28]([CH3:29])([CH3:30])[S:31]([NH2:32])(=[O:33])=[O:34])[c:23]3[c:22]2[cH:21][cH:20]1.OB(O)[c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10]...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O.OB(O)c1ccccc1
CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CCCC(C)(C)S(N)(=O)=O
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
89ee2e97ba79660eddf3dfa788334e60a83082a3d4afa6ed050c5f1f85789150
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3c(c2)ncc2nc[nH]c23)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)-[c;H0;D3;+0:13](:[c:14]:[c:15]):[c:16]:[c:17]>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13](:[c:14]:[c:15]):[c:16]:[c:17]):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1:[#7;a:7]
20.8
[{"value": 20.8, "product": "CC(CCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C2=CC=CC=C2)N)COCC)(S(=O)(=O)N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Dimethyl 4-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)butane-1-sulfonamide (0.66 g, 1.4 mmol) and phenyl boronic acid (0.20 g, 1.6 mmol) were coupled according to the method described in Part J of Example 1. The reaction was heated at reflux for 14 hours, and the work-up procedure used in Part F of ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HBr.B
null
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)(C)S(N)(=O)=O.OB(O)c1ccccc1>>CCOCc1nc2c(N)nc3cc(-c4ccccc4)ccc3c2n1CCCC(C)(C)S(N)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-600bf3d103d74d4c8b6ec0893592398f
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O.OB(O)c1cccnc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O
COC1=CC=C(CC(CCCN2C(=NC=3C(=NC=4C=C(C=CC4C32)Br)N)COCC)S(=O)(=O)N)C=C1.N1=CC(=CC=C1)B(O)O.N1=CC(=CC=C1)B(O)O>>COC1=CC=C(CC(CCCN2C(=NC=3C(=NC=4C=C(C=CC4C32)C=3C=NC=CC3)N)COCC)S(=O)(=O)N)C=C1
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:24]([CH2:25][CH2:26][CH2:27][CH:28]([CH2:29][c:30]4[cH:31][cH:32][c:33]([O:34][CH3:35])[cH:36][cH:37]4)[S:38]([NH2:39])(=[O:40])=[O:41])[c:23]3[c:22]2[cH:21][cH:20]1.OB(O)[c:14]1[cH:15][cH:16][cH:17][n:18][cH:19]1>>[CH3:1][CH2:2][...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O.OB(O)c1cccnc1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
d23a08b59b246d837a860414fc085402a8d785d2b981e3447d503da913f098ed
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(CCCCCn2cnc3cnc4cc(-c5cccnc5)ccc4c32)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)-[c;H0;D3;+0:13]1:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]3:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1...
53.9
[{"value": 53.9, "product": "COC1=CC=C(CC(CCCN2C(=NC=3C(=NC=4C=C(C=CC4C32)C=3C=NC=CC3)N)COCC)S(=O)(=O)N)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Methoxybenzyl 4-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)butane-1-sulfonamide (1.16 g, 2.0 mmol) and pyridine-3-boronic acid (0.30 g, 2.4 mmol) were coupled according to the method described in Part J of Example 1. The reaction was heated at reflux for 14 hours, at which time additional pyridine...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.c1ccccc1
HBr.B
null
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O.OB(O)c1cccnc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-24b232e9b29f4e4097636a3ef525cd72
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCS(N)(=O)=O
COC1=CC=C(CC(CCCN2C(=NC=3C(=NC=4C=C(C=CC4C32)C=3C=NC=CC3)N)COCC)S(=O)(=O)N)C=C1>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCS(=O)(=O)N)COCC)C=2C=NC=CC2
COc1ccc(C[CH:28]([CH2:27][CH2:26][CH2:25][n:24]2[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]3[c:8]([NH2:9])[n:10][c:11]4[cH:12][c:13](-[c:14]5[cH:15][cH:16][cH:17][n:18][cH:19]5)[cH:20][cH:21][c:22]4[c:23]32)[S:29]([NH2:30])(=[O:31])=[O:32])cc1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:1...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCS(N)(=O)=O
null
null
FC(C(=O)O)(F)F
Reduction
OtherReaction
37db49c452d6ff08df3eff3ac1188585096100b032f2fef99660b7108114c4fd
84394d34c591024a84d9393eb3e8adb8ada5a6225c3abafc4dae9aedd4568be4
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
C-O-c1:c:c:c(-C-[CH;D3;+0:1](-[C:2]-[C:3])-[#16:4](-[N;D1;H2:5])(=[O;D1;H0:6])=[O;D1;H0:7]):c:c:1>>[C:3]-[C:2]-[CH2;D2;+0:1]-[#16:4](-[N;D1;H2:5])(=[O;D1;H0:6])=[O;D1;H0:7]
77.5
[{"value": 77.5, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCS(=O)(=O)N)COCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A solution of 4-methoxybenzyl 4-[4-amino-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-1-yl]butane-1-sulfonamide (0.50 g, 0.88 mmol) in trifluoroacetic acid (5 mL) was stirred at ambient temperature for four hours and then concentrated under reduced pressure. The residue was dissolved in methanol and concen...
10.6084/m9.figshare.5104873.v1
null
Ether
null
c1ccccc1
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HO-
FC(C(=O)O)(F)F
null
0.5
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(Cc1ccc(OC)cc1)S(N)(=O)=O>FC(C(=O)O)(F)F>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCS(N)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-db20c0a683854d36b57eabfee6614a32
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)S(N)(=O)=O.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(C)S(N)(=O)=O
CC(CCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)S(=O)(=O)N.B1(OCCCO1)C2=CN=CC=C2.B1(OCCCO1)C2=CN=CC=C2.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>CC(CCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)S(=O)(=O)N
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:24]([CH2:25][CH2:26][CH2:27][CH:28]([CH3:29])[S:30]([NH2:31])(=[O:32])=[O:33])[c:23]3[c:22]2[cH:21][cH:20]1.C1COB([c:14]2[cH:15][cH:16][cH:17][n:18][cH:19]2)OC1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)S(N)(=O)=O.c1cncc(B2OCCCO2)c1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(C)S(N)(=O)=O
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
null
C-C Coupling
Suzuki coupling with boronic esters
2cd1cbe6f17c98cb5223a75d20dfc144a6eae8461c4fe8a7e9cc4bc7ecadb166
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.C1-C-O-B(-[c;H0;D3;+0:13]2:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:2)-O-C-1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]3:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5...
97.9
[{"value": 97.9, "product": "CC(CCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)S(=O)(=O)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Methyl 4-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)butane-1-sulfonamide (0.78 g, 1.7 mmol) and pyridine-3-boronic acid 1,3-propanediol cyclic ester (0.33 g, 2.0 mmol) were coupled according to the method described in Part J of Example 1. The reaction was heated at reflux for 15 hours, at which time...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccc2c(c1)ncc1[nH]cnc12.B1OCCCO1.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HBr.B
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCC(C)S(N)(=O)=O.c1cncc(B2OCCCO2)c1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCC(C)S(N)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-45a57d7b811b4b1789a26203d86721d9
O=S(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCO>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCCl
O.S(=O)(Cl)Cl.BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCCCO.C([O-])(O)=O.[Na+]>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCCCCCl
O=S(Cl)[Cl:21].O[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][NH:15][c:14]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]21>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:6][c:7]2[cH:8][c:9]([Br:10])[cH:11][cH:12][c:13]2[c:14]1[NH:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][Cl:21]
O=S(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCO
O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCCl
null
null
ClCCl
Functional Group Interconversion
Alcohol to chloride_SOCl2
bb752b9027dc4488ba075e5955118a819f80cabd751a7497b67c2eeb1db6b071
cbf41c7cf9fe6b47a243b1674d74ed5bf46a151f7f3a71d206e23176e158facf
c1ccc2ncccc2c1
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3]-[C:4]>>[C:4]-[C:3]-[CH2;D2;+0:2]-[Cl;H0;D1;+0:1]
null
[]
0
CELSIUS
5
MINUTE
A suspension of 5-(7-bromo-3-nitroquinolin-4-ylamino)pentan-1-ol (0.92 g, 2.6 mmol) in dichloromethane (13 mL) was cooled to 0° C.; thionyl chloride was added dropwise. The reaction was stirred for five minutes at 0° C. then allowed to warm to ambient temperature and stirred overnight. Saturated aqueous sodium bicarbon...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Primary halide
null
null
c1ccc2ncccc2c1
HCl
ClCCl
0
0.083333
O=S(Cl)Cl.O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCO>ClCCl>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCCCCCCl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d3476380362741e8b181f688fb0be9e4
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCCl.NC(N)=S>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCSC(=N)N.Cl
NC(=S)N.[I-].[K+].BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCCCl)COCC>>Cl.BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCCSC(N)=N)COCC
[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][Cl:28].[S:24]=[C:25]([NH2:26])[NH2:27]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH...
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCCl.NC(N)=S
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCSC(=N)N.Cl
null
null
CN(C)C=O
Protection
OtherReaction
dae623ec10e42086cc0292009bc19d7d58877ce2428714b92cfbbb5102c39de2
f72dba6c0cce6a796ff9aeda8637cc446706f96a34b889e05557c4a922c09746
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[C:2]-[CH2;D2;+0:3]-[Cl;H0;D1;+0:4].[N;D1;H2:5]-[C;H0;D3;+0:6](-[NH2;D1;+0:7])=[S;H0;D1;+0:8]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[S;H0;D2;+0:8]-[C;H0;D3;+0:6](-[N;D1;H2:5])=[NH;D1;+0:7].[ClH;D0;+0:4]
95.6
[{"value": 95.6, "product": "Cl.BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCCSC(N)=N)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
110
CELSIUS
null
null
Thiourea (0.29 g, 3.8 mmol) and potassium iodide (0.052 g, 3.1 mmol) were sequentially added to a suspension of 7-bromo-1-(5-chloropentyl)-2-ethoxymethyl-1H-imidazo[4,5-c]quinoline (1.3 g, 3.2 mmol) in DMF (15 mL), and the reaction was heated at 110° C. for 24 hours. The DMF was removed under reduced pressure, and the ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Thiourea
Monosulfide
null
null
c1ccc2c(c1)ncc1[nH]cnc12
null
CN(C)C=O
110
null
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCCl.NC(N)=S>CN(C)C=O>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCSC(=N)N.Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f632421fc58442f9bc72226e808ac80b
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCSC(=N)N.Cl.O>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCS(=O)(=O)Cl
Cl.BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCCSC(N)=N)COCC.Cl(=O)(=O)[O-].[Na+].O>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCCCCS(=O)(=O)Cl)COCC
N=C(N)[S:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][n:18]1[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]21.[ClH:27].[OH2:26]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][C...
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCSC(=N)N.Cl.O
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCS(=O)(=O)Cl
null
null
Cl
Oxidation
OtherReaction
c8e4f0823fd5da6f26236fd3ee99987b5fb983faa69924c535f5f775905feeb8
27319d95a096e5d4d5b1b326e21b5809676e06374d8e8d8ebb8a310f3ca2eedf
c1ccc2c(c1)ncc1nc[nH]c12
N-C(=N)-[S;H0;D2;+0:1]-[C:2]-[C:3].[ClH;D0;+0:4].[OH2;D0;+0:5]>>[C:3]-[C:2]-[S;H0;D4;+0:1](-[Cl;H0;D1;+0:4])(=[O;D1;H0:6])=[O;H0;D1;+0:5]
null
[]
null
null
null
null
A solution of 2-[5-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)pentyl]isothiourea hydrochloride (1.49 g, 3.16 mmol) in 7 M hydrochloric acid (8 mL) was cooled to 0° C. A solution of sodium chlorate (0.44 g, 4.1 mmol) in water (1.0 mL) was added dropwise with stirring, and the reaction was stirred at 0° C. fo...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Monosulfide
Sulfonyl halide
null
null
c1ccc2c(c1)ncc1[nH]cnc12
Other
Cl
null
null
CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCSC(=N)N.Cl.O>Cl>CCOCc1nc2cnc3cc(Br)ccc3c2n1CCCCCS(=O)(=O)Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0cf36a9b9fe846209e97efb76af17162
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCC(C)(C)S(N)(=O)=O.OB(O)c1cccnc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCC(C)(C)S(N)(=O)=O
CC(CCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)(S(=O)(=O)N)C.N1=CC(=CC=C1)B(O)O.N1=CC(=CC=C1)B(O)O>>CC(CCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)(S(=O)(=O)N)C
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:24]([CH2:25][CH2:26][CH2:27][CH2:28][C:29]([CH3:30])([CH3:31])[S:32]([NH2:33])(=[O:34])=[O:35])[c:23]3[c:22]2[cH:21][cH:20]1.OB(O)[c:14]1[cH:15][cH:16][cH:17][n:18][cH:19]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9]...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCC(C)(C)S(N)(=O)=O.OB(O)c1cccnc1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCC(C)(C)S(N)(=O)=O
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
null
C-C Coupling
Suzuki coupling with boronic acids
d23a08b59b246d837a860414fc085402a8d785d2b981e3447d503da913f098ed
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)-[c;H0;D3;+0:13]1:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]3:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1...
34.2
[{"value": 34.2, "product": "CC(CCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)(S(=O)(=O)N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
14
HOUR
Dimethyl 5-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)pentane-1-sulfonamide (0.26 g, 0.53 mmol) and pyridine-3-boronic acid (0.78 g, 0.63 mmol) were coupled according to the method described in Part J of Example 1. The reaction was heated at 100° C. for 31 hours, at which time additional palladium a...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HBr.B
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
null
14
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCC(C)(C)S(N)(=O)=O.OB(O)c1cccnc1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCC(C)(C)S(N)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ce7e2c982b6d4f79bcb6c0ac461bd472
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCC(C)S(N)(=O)=O.OB(O)c1cccnc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCC(C)S(N)(=O)=O
CC(CCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)S(=O)(=O)N.N1=CC(=CC=C1)B(O)O>>CC(CCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)S(=O)(=O)N
Br[c:13]1[cH:12][c:11]2[n:10][c:8]([NH2:9])[c:7]3[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:24]([CH2:25][CH2:26][CH2:27][CH2:28][CH:29]([CH3:30])[S:31]([NH2:32])(=[O:33])=[O:34])[c:23]3[c:22]2[cH:21][cH:20]1.OB(O)[c:14]1[cH:15][cH:16][cH:17][n:18][cH:19]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCC(C)S(N)(=O)=O.OB(O)c1cccnc1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCC(C)S(N)(=O)=O
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
d23a08b59b246d837a860414fc085402a8d785d2b981e3447d503da913f098ed
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.O-B(-O)-[c;H0;D3;+0:13]1:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]3:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1...
27.8
[{"value": 27.8, "product": "CC(CCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)S(=O)(=O)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Methyl 5-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)pentane-1-sulfonamide (0.47 g, 0.97 mmol) was coupled with pyridine-3-boronic acid (0.14 g, 1.2 mmol) according to the methods described in Part J of Example 1 and Part H of Example 370. The crude product was purified twice by HPFC (eluting with ch...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HBr.B
null
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCC(C)S(N)(=O)=O.OB(O)c1cccnc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCC(C)S(N)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-17aa753a322d4484be062a0385310189
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)OC(C)(C)C>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(OC(C)(C)C)=O)COCC)C=2C=NC=CC2>>NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC
CC(C)(C)OC(=O)[NH:29][CH2:28][CH2:27][CH2:26][CH2:25][n:24]1[c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][cH:17][n:18][cH:19]4)[cH:20][cH:21][c:22]3[c:23]21>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)OC(C)(C)C
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN
null
null
Cl
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
113.6
[{"value": 113.6, "product": "NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
A solution of tert-butyl {4-[4-amino-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-1-yl]butyl}carbamate (40.35 g, 82.24 mmol) in concentrated hydrochloric acid (400 mL) was stirred for one hour, filtered, and concentrated under reduced pressure. The residue was dissolved in a minimal amount of water, and 50...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HO-
Cl
null
0.5
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)OC(C)(C)C>Cl>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8286c1f00f7142c681fea48b02e013db
CCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)OC(C)(C)C>>CCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN
C([O-])(O)=O.[Na+].C([O-])([O-])=O.[Na+].[Na+].NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(OC(C)(C)C)=O)CCC)C=2C=NC=CC2.[OH-].[Na+].[Cl-].[Na+]>>NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)CCC
CC(C)(C)OC(=O)[NH:28][CH2:27][CH2:26][CH2:25][CH2:24][n:23]1[c:4]([CH2:3][CH2:2][CH3:1])[n:5][c:6]2[c:7]([NH2:8])[n:9][c:10]3[cH:11][c:12](-[c:13]4[cH:14][cH:15][cH:16][n:17][cH:18]4)[cH:19][cH:20][c:21]3[c:22]21>>[CH3:1][CH2:2][CH2:3][c:4]1[n:5][c:6]2[c:7]([NH2:8])[n:9][c:10]3[cH:11][c:12](-[c:13]4[cH:14][cH:15][cH:16...
CCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)OC(C)(C)C
CCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN
null
null
C(Cl)(Cl)Cl.Cl
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
87
[{"value": 87.0, "product": "NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of tert-butyl {4-[4-amino-2-propyl-7-(pyridin-3-yl)-1H-imidazol[4,5-c]quinolin-1-yl]butyl}carbamate (41.92 g, 88.32 mmol) in concentrated hydrochloric acid (210 mL) was stirred for ten minutes, and 50% aqueous sodium hydroxide was added to adjust the solution to pH 14. Cloroform (2.0 L) and a mixture of satu...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HO-
C(Cl)(Cl)Cl.Cl
null
8
CCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)OC(C)(C)C>C(Cl)(Cl)Cl.Cl>CCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4c81e4ee6509425ba1349d592b141c5f
CC(C)(C)OC(=O)NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>CC(C)(C)OC(=O)NCCNc1c(N)cnc2cc(Br)ccc12
C(C)(C)(C)OC(NCCNC1=C(C=NC2=CC(=CC=C12)Br)[N+](=O)[O-])=O.C(C)(C)O>>NC=1C=NC2=CC(=CC=C2C1NCCNC(OC(C)(C)C)=O)Br
O=[N+:14]([O-])[c:13]1[c:12]([NH:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[c:23]2[c:17]([n:16][cH:15]1)[cH:18][c:19]([Br:20])[cH:21][cH:22]2>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][NH:11][c:12]1[c:13]([NH2:14])[cH:15][n:16][c:17]2[cH:18][c:19]([Br:20])[cH:2...
CC(C)(C)OC(=O)NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
CC(C)(C)OC(=O)NCCNc1c(N)cnc2cc(Br)ccc12
null
[Pt]
C(C)#N
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2ncccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
91.1
[{"value": 91.1, "product": "NC=1C=NC2=CC(=CC=C2C1NCCNC(OC(C)(C)C)=O)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of tert-butyl[2-(7-bromo-3-nitroquinolin-4-ylamino)ethyl]carbamate (165.0 g, 401.2 mmol) in acetonitrile (3.3 L) and, isopropanol (990 mL) and 5% platinum on carbon (13.2 g) were added to a Parr vessel, which was placed under hydrogen pressure (50 psi, 3.4×105 Pa) overnight. The mixture was filtered through ...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C(C)#N
null
null
CC(C)(C)OC(=O)NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>[Pt].C(C)#N>CC(C)(C)OC(=O)NCCNc1c(N)cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b4129340568849b5959a9ea21a3b9236
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNC(=O)OC(C)(C)C.OB(O)c1cccnc1>>CCOCc1nc2cnc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)OC(C)(C)C
C(C)(C)(C)OC(NCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)=O.N1=CC(=CC=C1)B(O)O>>C(C)OCC=1N(C2=C(C=NC=3C=C(C=CC23)C=2C=NC=CC2)N1)CCNC(OC(C)(C)C)=O
N[c:8]1[c:7]2[n:6][c:5]([CH2:4][O:3][CH2:2][CH3:1])[n:23]([CH2:24][CH2:25][NH:26][C:27](=[O:28])[O:29][C:30]([CH3:31])([CH3:32])[CH3:33])[c:22]2[c:21]2[c:10]([n:9]1)[cH:11][c:12](Br)[cH:19][cH:20]2.OB(O)[c:13]1[cH:14][cH:15][cH:16][n:17][cH:18]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][c:12...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNC(=O)OC(C)(C)C.OB(O)c1cccnc1
CCOCc1nc2cnc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)OC(C)(C)C
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
C1(=CC=CC=C1)C
C-C Coupling
OtherReaction
e9d881b426c9c0b8a93a40293c3d0b6c34b426c55c2d9cabdc9aa863bd3d8244
79fc43732b29814f22dd0a7cbc24a0ef705cb8e808911cfb2a64a2630fa44903
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c;H0;D3;+0:5](-N):[c:6]3:[#7;a:7]:[c:8]:[#7;a:9](-[C:10]):[c:11]:3:[c:12]:2:[c:13]:[c:14]:1.O-B(-O)-[c;H0;D3;+0:15]1:[c:16]:[c:17]:[c:18]:[#7;a:19]:[c:20]:1>>[C:10]-[#7;a:9]1:[c:8]:[#7;a:7]:[c:6]2:[cH;D2;+0:5]:[#7;a:4]:[c:3]3:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:15]4:[c:16]:[c:17]...
51.4
[{"value": 51.4, "product": "C(C)OCC=1N(C2=C(C=NC=3C=C(C=CC23)C=2C=NC=CC2)N1)CCNC(OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
tert-Butyl[2-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethyl]carbamate (21.80 g, 46.94 mmol) and 3-pyridylboronic acid (6.64 g, 54.0 mmol) were coupled according to the method described in Part J of Example 1. Palladium (II) acetate was added as a 5 mg/mL solution in toluene. The reaction was termi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HBr.B
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)C
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNC(=O)OC(C)(C)C.OB(O)c1cccnc1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)C>CCOCc1nc2cnc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-300f431f77bb4ac1863898c99805673a
CC(C)C(=O)Cl.CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)C(C)C
NCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC.C(C)N(CC)CC.C(C(C)C)(=O)Cl>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNC(C(C)C)=O)COCC)C=2C=NC=CC2
Cl[C:28](=[O:29])[CH:30]([CH3:31])[CH3:32].[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][cH:17][n:18][cH:19]4)[cH:20][cH:21][c:22]3[c:23]2[n:24]1[CH2:25][CH2:26][NH2:27]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:...
CC(C)C(=O)Cl.CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)C(C)C
null
null
null
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])-[C;D1;H3:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])-[C;D1;H3:5]
32.8
[{"value": 32.8, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNC(C(C)C)=O)COCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
1-(2-Aminoethyl)-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine (2.00 g, 5.50 mmol) was treated with triethylamine (1.00 mL, 7.20 mmol) and isobutyryl chloride (0.64 mL, 6.10 mmol) according to the method described in Part B of Examples 372–376. The crude product was recrystallized from 93:7 acetonit...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HCl
null
null
null
CC(C)C(=O)Cl.CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)C(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f821a871b0c34016a9207fe1cb068308
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN.CS(=O)(=O)Cl>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNS(C)(=O)=O
CS(=O)(=O)Cl.NCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC.C(C)N(CC)CC.CS(=O)(=O)Cl.O>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNS(=O)(=O)C)COCC)C=2C=NC=CC2
[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][cH:17][n:18][cH:19]4)[cH:20][cH:21][c:22]3[c:23]2[n:24]1[CH2:25][CH2:26][NH2:27].Cl[S:28]([CH3:29])(=[O:30])=[O:31]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN.CS(=O)(=O)Cl
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNS(C)(=O)=O
null
null
C(Cl)(Cl)Cl
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:5]-[C:6]-[NH;D2;+0:7]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
26.8
[{"value": 26.8, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNS(=O)(=O)C)COCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
A solution of 1-(2-aminoethyl)-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine (2.00 g, 5.50 mmol) in chloroform (40 mL) was treated with triethylamine (1.62 mL, 11.6 mmol) and methanesulfonyl chloride (0.47 mL, 6.05 mmol). The reaction was stirred for 1.5 hours, and additional methanesulfonyl chlorid...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HCl
C(Cl)(Cl)Cl
null
1.5
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN.CS(=O)(=O)Cl>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d16d8d902d0c45cfb7ea9fa85a26dbda
CC(C)N=C=O.CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)NC(C)C
NCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC.C(C)(C)N=C=O>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNC(=O)NC(C)C)COCC)C=2C=NC=CC2
[C:28](=[O:29])=[N:30][CH:31]([CH3:32])[CH3:33].[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][cH:17][n:18][cH:19]4)[cH:20][cH:21][c:22]3[c:23]2[n:24]1[CH2:25][CH2:26][NH2:27]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13]...
CC(C)N=C=O.CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)NC(C)C
null
null
C(Cl)(Cl)Cl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
[C;D1;H3:1]-[C:2](-[C;D1;H3:3])-[N;H0;D2;+0:4]=[C;H0;D2;+0:5]=[O;D1;H0:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[C;H0;D3;+0:5](=[O;D1;H0:6])-[NH;D2;+0:4]-[C:2](-[C;D1;H3:1])-[C;D1;H3:3]
28.5
[{"value": 28.5, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNC(=O)NC(C)C)COCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 1-(2-aminoethyl)-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine (2.50 g, 6.90 mmol) in chloroform (50 mL) was treated with isopropyl isocyanate (0.65 mL, 6.9 mmol) according to the method described in Examples 377–379. The crude product was purified by column chromatography on silica ge...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
null
C(Cl)(Cl)Cl
null
null
CC(C)N=C=O.CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)NC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bd2e3b5bb7384ffca222305e95fc44cb
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNC(=O)OC(C)(C)C.OB(O)c1cccnc1>>CCCCc1nc2cnc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)OC(C)(C)C
C(C)(C)(C)OC(NCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)CCCC)=O.N1=CC(=CC=C1)B(O)O>>C(C)(C)(C)OC(NCCN1C(=NC=2C=NC=3C=C(C=CC3C21)C=2C=NC=CC2)CCCC)=O
N[c:8]1[c:7]2[n:6][c:5]([CH2:4][CH2:3][CH2:2][CH3:1])[n:23]([CH2:24][CH2:25][NH:26][C:27](=[O:28])[O:29][C:30]([CH3:31])([CH3:32])[CH3:33])[c:22]2[c:21]2[c:10]([n:9]1)[cH:11][c:12](Br)[cH:19][cH:20]2.OB(O)[c:13]1[cH:14][cH:15][cH:16][n:17][cH:18]1>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[cH:8][n:9][c:10]3[cH:11][...
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNC(=O)OC(C)(C)C.OB(O)c1cccnc1
CCCCc1nc2cnc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)OC(C)(C)C
null
null
null
C-C Coupling
OtherReaction
e9d881b426c9c0b8a93a40293c3d0b6c34b426c55c2d9cabdc9aa863bd3d8244
79fc43732b29814f22dd0a7cbc24a0ef705cb8e808911cfb2a64a2630fa44903
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c;H0;D3;+0:5](-N):[c:6]3:[#7;a:7]:[c:8]:[#7;a:9](-[C:10]):[c:11]:3:[c:12]:2:[c:13]:[c:14]:1.O-B(-O)-[c;H0;D3;+0:15]1:[c:16]:[c:17]:[c:18]:[#7;a:19]:[c:20]:1>>[C:10]-[#7;a:9]1:[c:8]:[#7;a:7]:[c:6]2:[cH;D2;+0:5]:[#7;a:4]:[c:3]3:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:15]4:[c:16]:[c:17]...
83.2
[{"value": 83.2, "product": "C(C)(C)(C)OC(NCCN1C(=NC=2C=NC=3C=C(C=CC3C21)C=2C=NC=CC2)CCCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
tert-Butyl[2-(4-amino-7-bromo-2-butyl-1H-imidazo[4,5-c]quinolin-1-yl)ethyl]carbamate (14.09 g, 30.5 mmol) and 3-pyridylboronic acid (4.31 g, 35.0 mmol) were coupled according to the method described in Part G of Example 386. The reaction was heated for 2.5 hours. The crude product was triturated with toluene (15 mL/g) ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine.Boronic acid
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HBr.B
null
null
null
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNC(=O)OC(C)(C)C.OB(O)c1cccnc1>>CCCCc1nc2cnc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d4a7e716ac644acf804bc7c29619114a
CC(C)C(=O)Cl.CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN>>CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)C(C)C
NCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)CCCC.C(C)N(CC)CC.C(C(C)C)(=O)Cl>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNC(C(C)C)=O)CCCC)C=2C=NC=CC2
Cl[C:28](=[O:29])[CH:30]([CH3:31])[CH3:32].[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][cH:17][n:18][cH:19]4)[cH:20][cH:21][c:22]3[c:23]2[n:24]1[CH2:25][CH2:26][NH2:27]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](...
CC(C)C(=O)Cl.CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN
CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)C(C)C
null
null
null
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])-[C;D1;H3:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])-[C;D1;H3:5]
25.8
[{"value": 25.8, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNC(C(C)C)=O)CCCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
1-(2-Aminoethyl)-2-butyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine (2.00 g, 5.50 mmol) was treated with triethylamine (1.01 mL, 7.26 mmol) and isobutyryl chloride (0.64 mL, 6.10 mmol) according to the method described in Part B of Examples 372–376. The crude product was recrystallized from isopropanol (4 mL/g)...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HCl
null
null
null
CC(C)C(=O)Cl.CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN>>CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)C(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3db7633c7790473bbf510fa12aa014cc
CC(C)N=C=O.CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN>>CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)NC(C)C
C(C)(C)N=C=O.NCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)CCCC>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNC(=O)NC(C)C)CCCC)C=2C=NC=CC2
[C:28](=[O:29])=[N:30][CH:31]([CH3:32])[CH3:33].[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c:13](-[c:14]4[cH:15][cH:16][cH:17][n:18][cH:19]4)[cH:20][cH:21][c:22]3[c:23]2[n:24]1[CH2:25][CH2:26][NH2:27]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][c...
CC(C)N=C=O.CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN
CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)NC(C)C
null
null
C(Cl)(Cl)Cl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
c1cncc(-c2ccc3c(c2)ncc2nc[nH]c23)c1
[C;D1;H3:1]-[C:2](-[C;D1;H3:3])-[N;H0;D2;+0:4]=[C;H0;D2;+0:5]=[O;D1;H0:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[C;H0;D3;+0:5](=[O;D1;H0:6])-[NH;D2;+0:4]-[C:2](-[C;D1;H3:1])-[C;D1;H3:3]
47.8
[{"value": 47.8, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNC(=O)NC(C)C)CCCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Isopropyl isocyanate (0.29 mL, 3.1 mmol) was added slowly to a suspension of 1-(2-aminoethyl)-2-butyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine (1.13 g, 3.1 mmol) in chloroform (113 mL). A precipitate formed within 15 minutes, was isolated by filtration, and was dried overnight in an oven to provide 0.66 g of ...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
null
C(Cl)(Cl)Cl
null
null
CC(C)N=C=O.CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN>C(Cl)(Cl)Cl>CCCCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCNC(=O)NC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9ba31f07c1b444a68ce2aed691763f55
CC(C)(C)OC(=O)N1CCC(CNc2c(N)cnc3cc(Br)ccc23)CC1.CCOC(CC)(OCC)OCC>>CCc1nc2cnc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
NC=1C=NC2=CC(=CC=C2C1NCC1CCN(CC1)C(=O)OC(C)(C)C)Br.C(CC)(OCC)(OCC)OCC>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC3CCN(CC3)C(=O)OC(C)(C)C)CC
[NH2:4][c:5]1[cH:6][n:7][c:8]2[cH:9][c:10]([Br:11])[cH:12][cH:13][c:14]2[c:15]1[NH:16][CH2:17][CH:18]1[CH2:19][CH2:20][N:21]([C:22](=[O:23])[O:24][C:25]([CH3:26])([CH3:27])[CH3:28])[CH2:29][CH2:30]1.CCO[C:3](OCC)(OCC)[CH2:2][CH3:1]>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[cH:6][n:7][c:8]3[cH:9][c:10]([Br:11])[cH:12][cH:13][c:1...
CC(C)(C)OC(=O)N1CCC(CNc2c(N)cnc3cc(Br)ccc23)CC1.CCOC(CC)(OCC)OCC
CCc1nc2cnc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
8d87c769e65778c9400c7f523e0409ecf0ffad86543cd9fdd6ef4b239323db96
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc2c(c1)ncc1ncn(CC3CCNCC3)c12
C-C-O-[C;H0;D4;+0:1](-O-C-C)(-O-C-C)-[C:2]-[C;D1;H3:3].[C:4]-[C:5]-[NH;D2;+0:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:1-[NH2;D1;+0:13]>>[C:4]-[C:5]-[n;H0;D3;+0:6]1:[c:7]2:[c:8]:[c:9]:[#7;a:10]:[c:11]:[c:12]:2:[n;H0;D2;+0:13]:[c;H0;D3;+0:1]:1-[C:2]-[C;D1;H3:3]
77.1
[{"value": 77.1, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC3CCN(CC3)C(=O)OC(C)(C)C)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The method described in Part A of Examples 142–144 was used to treat tert-butyl 4-[(3-amino-7-bromoquinolin-4-ylamino)methyl]piperidine-1-carboxylate (15.0 g, 34.5 mmol) with triethyl orthopropionate (6.68 g, 37.9 mmol). After completion, the reaction mixture was concentrated under reduced pressure, and the residue was...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.C1CC[NH]CC1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(CNc2c(N)cnc3cc(Br)ccc23)CC1.CCOC(CC)(OCC)OCC>>CCc1nc2cnc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6ab58770b4c24ae7b57719be753f7eac
CCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1.c1cncc(B2OCCCO2)c1>>CCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2CCN(CC2)C(=O)OC(C)(C)C)CC)Br.B1(OCCCO1)C2=CN=CC=C2>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2CCN(CC2)C(=O)OC(C)(C)C)CC)C=2C=NC=CC2
Br[c:11]1[cH:10][c:9]2[n:8][c:6]([NH2:7])[c:5]3[n:4][c:3]([CH2:2][CH3:1])[n:22]([CH2:23][CH:24]4[CH2:25][CH2:26][N:27]([C:28](=[O:29])[O:30][C:31]([CH3:32])([CH3:33])[CH3:34])[CH2:35][CH2:36]4)[c:21]3[c:20]2[cH:19][cH:18]1.C1COB([c:12]2[cH:13][cH:14][cH:15][n:16][cH:17]2)OC1>>[CH3:1][CH2:2][c:3]1[n:4][c:5]2[c:6]([NH2:7...
CCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1.c1cncc(B2OCCCO2)c1
CCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
null
null
O
C-C Coupling
Suzuki coupling with boronic esters
2cd1cbe6f17c98cb5223a75d20dfc144a6eae8461c4fe8a7e9cc4bc7ecadb166
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1cncc(-c2ccc3c(c2)ncc2ncn(CC4CCNCC4)c23)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[c:10]:2:[c:11]:[c:12]:1.C1-C-O-B(-[c;H0;D3;+0:13]2:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:2)-O-C-1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[c;H0;D3;+0:13]3:[c:14]:[c:15]:[c:16]:[#7;a:17]:[c:18]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5...
59.2
[{"value": 59.2, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2CCN(CC2)C(=O)OC(C)(C)C)CC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
tert-Butyl 4-[(4-amino-7-bromo-2-ethyl-1H-imidazo[4,5-c]quinolin-1-yl)methyl]piperidine-1-carboxylate (9.24 g, 18.9 mmol) and pyridine-3-boronic acid 1,3-propanediol cyclic ester (3.39 g, 20.8 mmol) were coupled according to the method described in Examples 118–121. Additional reagents were added after the reaction was...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccc2c(c1)ncc1[nH]cnc12.B1OCCCO1.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.C1CC[NH]CC1
HBr.B
O
null
16
CCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1.c1cncc(B2OCCCO2)c1>O>CCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1