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-825b576ec3824178b44550c35afa2831
CC(C)(C)OC(=O)N1CCC(CNc2c(N)cnc3cc(Br)ccc23)CC1.CCCC(OC)(OC)OC>>CCCc1nc2cnc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
NC=1C=NC2=CC(=CC=C2C1NCC1CCN(CC1)C(=O)OC(C)(C)C)Br.C(CCC)(OC)(OC)OC>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC3CCN(CC3)C(=O)OC(C)(C)C)CCC
[NH2:5][c:6]1[cH:7][n:8][c:9]2[cH:10][c:11]([Br:12])[cH:13][cH:14][c:15]2[c:16]1[NH:17][CH2:18][CH:19]1[CH2:20][CH2:21][N:22]([C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29])[CH2:30][CH2:31]1.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]([Br:12])[cH:1...
CC(C)(C)OC(=O)N1CCC(CNc2c(N)cnc3cc(Br)ccc23)CC1.CCCC(OC)(OC)OC
CCCc1nc2cnc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
8d87c769e65778c9400c7f523e0409ecf0ffad86543cd9fdd6ef4b239323db96
a60e703c3cf5c0d933aa031358d338c45d96ec82dec3fc2d9f5dce06b9dcc651
c1ccc2c(c1)ncc1ncn(CC3CCNCC3)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]
77.9
[{"value": 77.9, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC3CCN(CC3)C(=O)OC(C)(C)C)CCC", "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 trimethyl orthobutyrate (5.62 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.CCCC(OC)(OC)OC>>CCCc1nc2cnc3cc(Br)ccc3c2n1CC1CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ed6c6d0d8e3d4c479e339443c4683a34
CC(C)(C)OC(=O)N1CCN(CCN)CC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>CC(C)(C)OC(=O)N1CCN(CCNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)CC1
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.NCCN1CCN(CC1)C(=O)OC(C)(C)C>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCN1CCN(CC1)C(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([CH2:12][CH2:13][NH2:14])[CH2:29][CH2:30]1.Cl[c:15]1[c:16]([N+:17](=[O:18])[O-:19])[cH:20][n:21][c:22]2[cH:23][c:24]([Br:25])[cH:26][cH:27][c:28]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([CH2:12][CH2:13][NH...
CC(C)(C)OC(=O)N1CCN(CCN)CC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
CC(C)(C)OC(=O)N1CCN(CCNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)CC1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2c(NCCN3CCNCC3)ccnc2c1
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]
59.8
[{"value": 59.8, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCN1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
7-Bromo-4-chloro-3-nitroquinoline (33.0 g, 115 mmol) was treated with 4-(2-aminoethyl)-1-(tert-butoxycarbonyl)piperazine (26.4 mL, 115 mmol) according to the method described in Part E of Example 1. The reaction was stirred overnight. The crude product was triturated with diethyl ether and isolated by filtration to pro...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
C1C[NH]CC[NH]1.c1ccc2ncccc2c1
HCl
null
null
8
CC(C)(C)OC(=O)N1CCN(CCN)CC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>CC(C)(C)OC(=O)N1CCN(CCNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fde1062fb7e5468ca3c9b1d8f714ccd0
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC[N+]1([O-])CCN(C(=O)OC(C)(C)C)CC1.ClP(Cl)Cl>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCN1CCNCC1.Cl.Cl
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC[N+]2(CCN(CC2)C(=O)OC(C)(C)C)[O-])COCC)Br.P(Cl)(Cl)Cl>>Cl.Cl.BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CCN3CCNCC3)COCC
CC(C)(C)OC(=O)[N:25]1[CH2:24][CH2:23][N+:22]([O-])([CH2:21][CH2:20][n:19]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]([Br:14])[cH:15][cH:16][c:17]4[c:18]32)[CH2:27][CH2:26]1.ClP([Cl:28])[Cl:29]>>[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(Br)ccc3c2n1CC[N+]1([O-])CCN(C(=O)OC(C)(C)C)CC1.ClP(Cl)Cl
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCN1CCNCC1.Cl.Cl
null
O
C(Cl)(Cl)Cl
Miscellaneous
OtherReaction
baebd3535e3c3ed48ea5d112df2046b97d58245c6fb078b0192e50e124437cab
f6a4ae6324f8dbd1ee43b452848ffb52b7dc085d08b53e9c735ec57db6466f6c
c1ccc2c(c1)ncc1ncn(CCN3CCNCC3)c12
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[N+;H0;D4:4](-[O-])(-[C:5]-[C:6])-[C:7]-[C:8]-1.Cl-P(-[Cl;H0;D1;+0:9])-[Cl;H0;D1;+0:10]>>[C:6]-[C:5]-[N;H0;D3;+0:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:8]-[C:7]-1.[ClH;D0;+0:9].[ClH;D0;+0:10]
84.2
[{"value": 84.2, "product": "Cl.Cl.BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CCN3CCNCC3)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
4
CELSIUS
45
MINUTE
A solution of tert-butyl 4-[2-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)ethyl]-4-oxidopiperazine-1-carboxylate (8.84 g, 16.1 mmol) in chloroform (400 mL) was cooled to 4° C. Phosphorous trichloride (9.82 mL, 113 mmol) was added dropwise, and the reaction was stirred for 45 minutes at 4° C. Water (o...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine.Tertiary amine
C1C[NH+]CC[NH]1
C1C[NH]CCN1
c1ccc2c(c1)ncc1[nH]cnc12.C1C[NH]CCN1
HCl
O.C(Cl)(Cl)Cl
4
0.75
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC[N+]1([O-])CCN(C(=O)OC(C)(C)C)CC1.ClP(Cl)Cl>O.C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCN1CCNCC1.Cl.Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1be1f82b79c64a0c962f9a12b8547cb9
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCN1CCNCC1.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN1CCNCC1
O.C([O-])([O-])=O.[Na+].[Na+].Cl.Cl.BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CCN3CCNCC3)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)CCN1CCNCC1
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][N:27]4[CH2:28][CH2:29][NH:30][CH2:31][CH2:32]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:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12][...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCN1CCNCC1.c1cncc(B2OCCCO2)c1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN1CCNCC1
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1
C(CC)O.C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic esters
2cd1cbe6f17c98cb5223a75d20dfc144a6eae8461c4fe8a7e9cc4bc7ecadb166
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1cncc(-c2ccc3c(c2)ncc2ncn(CCN4CCNCC4)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...
78.9
[{"value": 78.9, "product": "C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CCN1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Under a nitrogen atmosphere, triphenylphosphine (0.0409 g, 0.156 mmol), 2 M aqueous sodium carbonate (18.3 mL, 36.5 mmol) and a solution of palladium (II) acetate (0.0117 g, 0.52 mmol) in warm toluene were added to a solution of 7-bromo-2-ethoxymethyl-1-(2-piperazin-1-ylethyl)-1H-imidazo[4,5-c]quinolin-4-amine dihydroc...
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.C1C[NH]CCN1
HBr.B
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(CC)O.C1(=CC=CC=C1)C
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCN1CCNCC1.c1cncc(B2OCCCO2)c1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(CC)O.C1(=CC=CC=C1)C>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCN1CCNCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dd064fe13c304d048f8985c83af1053f
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCCC(OC)(OC)OC>>CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
C(CCC)(OC)(OC)OC.Cl.N1=CC=CC=C1.NC=1C=NC2=CC(=CC=C2C1NCC(C)(O)C)Br>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)CCC
[NH2:5][c:6]1[cH:7][n:8][c:9]2[cH:10][c:11]([Br:12])[cH:13][cH:14][c:15]2[c:16]1[NH:17][CH2:18][C:19]([CH3:20])([CH3:21])[OH:22].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]([Br:12])[cH:13][cH:14][c:15]3[c:16]2[n:17]1[CH2:18][C:19]([CH3:20])([CH3:21])[OH:22]
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCCC(OC)(OC)OC
CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
null
null
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]
76.7
[{"value": 76.7, "product": "BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)(O)C)CCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Trimethyl orthobutyrate (11.61 mL, 72.6 mmol) and catalytic pyridine hydrochloride were added to a solution of 1-(3-amino-7-bromoquinolin-4-ylamino)-2-methylpropan-2-ol (22.51 g, 72.6 mmol) in anhydrous toluene (120 mL), and the reaction was heated at reflux for two hours. The solvent was removed under reduced pressure...
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-
C1(=CC=CC=C1)C
null
null
CC(C)(O)CNc1c(N)cnc2cc(Br)ccc12.CCCC(OC)(OC)OC>C1(=CC=CC=C1)C>CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)(C)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a0aab8bc0b124b31a57accf5057cc740
CC(C)Cn1cnc2c(N)nc3ccccc3c21.O=C1CCC(=O)N1Br>>CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
CC(CN1C=NC=2C(=NC=3C=CC=CC3C21)N)C.BrN1C(CCC1=O)=O>>BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)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][cH:15][cH:17][c:18]3[c:19]12.O=C1CCC(=O)N1[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][c:15]([Br:16])[cH:17][c:18]3[c:19]12
CC(C)Cn1cnc2c(N)nc3ccccc3c21.O=C1CCC(=O)N1Br
CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
null
null
C(Cl)(Cl)Cl
Functional Group Interconversion
Bromination
5d9faf536b16c566a8d6a04595b0f955faec3d2832e3b158ede2e30e6cf6e4a4
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccc2c(c1)ncc1nc[nH]c12
O=C1-C-C-C(=O)-N-1-[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]
22.6
[{"value": 22.6, "product": "BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A solution of 1-(2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine (30.0 g, 125 mmol) in chloroform (620 mL) was heated to 50° C., and N-bromosuccinimide (28.8 g, 162 mmol) was added in five portions over a period of five minutes. The resulting dark red solution was heated at reflux for 45 minutes, allowed to cool to a...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1nc2ccccc2c2[nH]cnc12.C1CCNC1
c1ccc2ncc3nc[nH]c3c2c1
c1ccc2ncc3nc[nH]c3c2c1
HO-
C(Cl)(Cl)Cl
null
1
CC(C)Cn1cnc2c(N)nc3ccccc3c21.O=C1CCC(=O)N1Br>C(Cl)(Cl)Cl>CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-06dcb0dc9288479ba77db93b0ebf51a7
C=Cc1ccncc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21>>CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccncc4)cc3c21
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C.C(=C)C1=CC=NC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(C)N(CC)CC>>CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)C=CC2=CC=NC=C2)N)C
[CH2:16]=[CH:17][c:18]1[cH:19][cH:20][n:21][cH:22][cH:23]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:26]3[c:25]2[cH:24]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]([CH:16]=[CH:17][c:18]4[cH:19][cH...
C=Cc1ccncc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccncc4)cc3c21
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
C(C)#N
C-C Coupling
Heck terminal vinyl
4d5b3e3981a57b3aeb73174e1869a0103c791712a7b3c712b27e875529a5446f
4b186811a4930853b446d93d9faa39b267bddb9ce0b8021bda5c5a3b2bc69f0b
C(=Cc1ccc2ncc3nc[nH]c3c2c1)c1ccncc1
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].[CH2;D1;+0:10]=[C:11]-[c:12]>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[CH;D2;+0:10]=[C:11]-[c:12]):[c:7]:[c:6]:1:[c:8]:[#7;a:9]
65.1
[{"value": 65.1, "product": "CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)C=CC2=CC=NC=C2)N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
Nitrogen was bubbled through a solution of 8-bromo-1-(2-methylpropyl)-1H-imidazo[4,5-c]-quinolin-4-amine (3.0 g, 9.4 mmol), 4-vinylpyridine (2.0 mL, 19 mmol), triphenylphosphine (246 mg, 0.94 mmol), and triethylamine (2.7 mL, 19 mmol) in acetonitrile (50 mL) for 15 minutes. Palladium (II) acetate (105 mg, 0.47 mmol) wa...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Vinyl
null
c1ccc2ncc3[nH]cnc3c2c1
c1ccc2ncc3nc[nH]c3c2c1
c1ccc2ncc3nc[nH]c3c2c1.c1ccncc1
HBr
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C(C)#N
100
null
C=Cc1ccncc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C(C)#N>CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccncc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-599b5e90987942499a26d367a008765e
CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccncc4)cc3c21>>CC(C)Cn1cnc2c(N)nc3ccc(CCc4ccncc4)cc3c21
CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)C=CC2=CC=NC=C2)N)C>>CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)CCC2=CC=NC=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][n: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:20...
CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccncc4)cc3c21
CC(C)Cn1cnc2c(N)nc3ccc(CCc4ccncc4)cc3c21
null
[Pd]
CO
Reduction
Hydrogenation (double to single)
0bc3968b35f0839c230afb4215314da278abd4e1f10e42ec3012c5512de49ea5
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1cc(CCc2ccc3ncc4nc[nH]c4c3c2)ccn1
[c:1]:[c:2](-[CH;D2;+0:3]=[CH;D2;+0:4]-[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1):[c:11]>>[c:1]:[c:2](-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1):[c:11]
18
[{"value": 18.0, "product": "CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)CCC2=CC=NC=C2)N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
7
DAY
1-(2-Methylpropyl)-8-(2-pyridin-4-ylvinyl)-1H-imidazo[4,5-c]-quinolin-4-amine (2.1 g, 6.1 mmol) was treated according to the method described in Example 123; the reaction was allowed to run for seven days. An analysis by proton nuclear magnetic resonance spectroscopy indicated the presence of starting material in the p...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccc2ncc3nc[nH]c3c2c1.c1ccncc1
null
[Pd].CO
null
168
CC(C)Cn1cnc2c(N)nc3ccc(C=Cc4ccncc4)cc3c21>[Pd].CO>CC(C)Cn1cnc2c(N)nc3ccc(CCc4ccncc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8018ff66f1b14643aeb0cf875f55bc8b
C=CCCc1ccccc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21>>CC(C)Cn1cnc2c(N)nc3ccc(C=CCCc4ccccc4)cc3c21
BrC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C.C1(=CC=CC=C1)CCC=C>>CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)C=CCCC2=CC=CC=C2)N)C
[CH2:16]=[CH:17][CH2:18][CH2:19][c:20]1[cH:21][cH:22][cH: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]([CH:16]=[CH:17]...
C=CCCc1ccccc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21
CC(C)Cn1cnc2c(N)nc3ccc(C=CCCc4ccccc4)cc3c21
null
null
null
C-C Coupling
OtherReaction
5c2a497c119c97c63096a3705db7c6fc998936207eb8d13d39dcfae27041b2b5
df8442c9f2045421fb18548edb9c6acaeb9710f63e741d9f72e0000ca35c948a
C(=Cc1ccc2ncc3nc[nH]c3c2c1)CCc1ccccc1
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].[C:10]-[C:11]=[CH2;D1;+0:12]>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[CH;D2;+0:12]=[C:11]-[C:10]):[c:7]:[c:6]:1:[c:8]:[#7;a:9]
51.7
[{"value": 51.7, "product": "CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)C=CCCC2=CC=CC=C2)N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
8-Bromo-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine (3.0 g, 9.4 mmol) was treated with 4-phenyl butene (4.2 mL, 28.2 mmol) according to the method described in Part B of Example 425. The reaction was heated overnight. Following chromatographic purification (eluting with 95:5 chloroform:methanol), 1.8 g of 1-(2...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Allyl
null
c1ccc2ncc3[nH]cnc3c2c1
c1ccc2ncc3nc[nH]c3c2c1
c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
HBr
null
null
null
C=CCCc1ccccc1.CC(C)Cn1cnc2c(N)nc3ccc(Br)cc3c21>>CC(C)Cn1cnc2c(N)nc3ccc(C=CCCc4ccccc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-aae0dad34e834b03a63c256ec63dadca
CC(C)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>CC(C)CNc1c(N)cnc2cc(Br)ccc12
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
[Pt]
C(C)(C)O.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]
null
[]
null
null
1
HOUR
A solution of (7-bromo-3-nitroquinolin-4-yl)-(2-methylpropyl)amine (30.9 g, 105 mmol) in acetonitrile (1.8 L) and isopropanol (200 mL) was added to a Parr vessel. A mixture of 5% platinum on carbon (3.0 g) and acetonitrile:isopropanol (20 mL) was added, and the vessel was purged with nitrogen. The vessel was placed und...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C(C)(C)O.C(C)#N
null
1
CC(C)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>[Pt].C(C)(C)O.C(C)#N>CC(C)CNc1c(N)cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-755d4f9ae9fc48b3bfbb003cb502e6b9
CC(C)Cn1cnc2cnc3cc(Br)ccc3c21.[NH4+]>>CC(C)Cn1cnc2c(N)nc3cc(Br)ccc3c21
BrC=1C=CC=2C3=C(C=NC2C1)N=CN3CC(C)C.ClC=1C=C(C(=O)OO)C=CC1.[OH-].[NH4+].C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>BrC=1C=CC=2C3=C(C(=NC2C1)N)N=CN3CC(C)C
[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[cH:9][n:11][c:12]3[cH:13][c:14]([Br:15])[cH:16][cH:17][c:18]3[c:19]12.[NH4+:10]>>[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][c:14]([Br:15])[cH:16][cH:17][c:18]3[c:19]12
CC(C)Cn1cnc2cnc3cc(Br)ccc3c21.[NH4+]
CC(C)Cn1cnc2c(N)nc3cc(Br)ccc3c21
null
null
C(C)#N
Functional Group Addition
OtherReaction
1b385f4f663d9a767870cf79c8a1cc13167a133dcf33a738d88383ea6a59da05
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
null
null
The method described in Part J of Example 365 was used to oxidize and aminate 7-bromo-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinoline (18.7 g, 58.4 mmol). 3-Chloroperoxybenzoic acid (22.1 g of 50% pure material, 129 mmol) was added in five portions during the oxidation step, and the amination with ammonium hydroxide (146...
10.6084/m9.figshare.5104873.v1
null
null
Primary amine
c1ccc2c(c1)ncc1nc[nH]c12
c1ccc2c(c1)ncc1nc[nH]c12
c1ccc2c(c1)ncc1nc[nH]c12
null
C(C)#N
null
null
CC(C)Cn1cnc2cnc3cc(Br)ccc3c21.[NH4+]>C(C)#N>CC(C)Cn1cnc2c(N)nc3cc(Br)ccc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f357290ac0064a0c9824d3f113be41d2
CC(C)Cn1cnc2c(N)nc3cc(C=Cc4ccccc4)ccc3c21>>CC(C)Cn1cnc2c(N)nc3cc(CCc4ccccc4)ccc3c21
CC(CN1C=NC=2C(=NC=3C=C(C=CC3C21)C=CC2=CC=CC=C2)N)C>>CC(CN1C=NC=2C(=NC=3C=C(C=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][c:14]([CH:15]=[CH:16][c:17]4[cH:18][cH:19][cH:20][cH:21][cH:22]4)[cH:23][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][c:14]([CH2:15][CH2:16][c:17]4[cH:18][cH:19][cH:2...
CC(C)Cn1cnc2c(N)nc3cc(C=Cc4ccccc4)ccc3c21
CC(C)Cn1cnc2c(N)nc3cc(CCc4ccccc4)ccc3c21
null
null
CO
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]
null
[]
null
null
null
null
A modification of the method described in Example 123 was used to reduce 1-(2-methylpropyl)-7-styryl-1H-imidazo[4,5-c]quinolin-4-amine (1.2 g, 3.5 mmol). The reaction was carried out in methanol (100 mL) for seven days. The crude product was purified by flash column chromatography on silica gel (eluting with 90:10 chlo...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccc2c(c1)ncc1nc[nH]c12.c1ccccc1
null
CO
null
null
CC(C)Cn1cnc2c(N)nc3cc(C=Cc4ccccc4)ccc3c21>CO>CC(C)Cn1cnc2c(N)nc3cc(CCc4ccccc4)ccc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1497b3ef15dc4b0aace9e821cdb10a10
CC1(C)OC(=O)CC(=O)O1.CCOC(OCC)OCC.Nc1ccc(Cc2ccccc2)cc1.Nc1cccc(Cc2ccccc2)c1>>CC1(C)OC(=O)C(=CNc2ccc(Cc3ccccc3)cc2)C(=O)O1.CC1(C)OC(=O)C(=CNc2cccc(Cc3ccccc3)c2)C(=O)O1
C(C1=CC=CC=C1)C=1C=C(N)C=CC1.C(OCC)(OCC)OCC.C(C1=CC=CC=C1)C1=CC=C(N)C=C1.CC1(OC(=O)CC(=O)O1)C>>C(C1=CC=CC=C1)C=1C=C(C=CC1)NC=C1C(OC(OC1=O)(C)C)=O.C(C1=CC=CC=C1)C1=CC=C(C=C1)NC=C1C(OC(OC1=O)(C)C)=O
[CH3:1][C:2]1([CH3:3])[O:4][C:5](=[O:6])[CH2:7][C:48](=[O:49])[O:25]1.[CH2:8]([CH3:23])[O:24][CH:33]([O:29][CH2:27][CH3:28])[O:31][CH2:30][CH3:32].[NH2:9][c:10]1[cH:11][cH:12][c:13]([CH2:14][c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[cH:21][cH:22]1.[NH2:34][c:35]1[cH:36][cH:37][cH:38][c:39]([CH2:40][c:41]2[cH:42][cH:4...
CC1(C)OC(=O)CC(=O)O1.CCOC(OCC)OCC.Nc1ccc(Cc2ccccc2)cc1.Nc1cccc(Cc2ccccc2)c1
CC1(C)OC(=O)C(=CNc2ccc(Cc3ccccc3)cc2)C(=O)O1.CC1(C)OC(=O)C(=CNc2cccc(Cc3ccccc3)c2)C(=O)O1
null
null
CO
Functional Group Addition
OtherReaction
c5e983f3b9e5026f979cb69feab0c38fb2eb5aa05407ae38d616c63063338bac
5c401633cc6fe8ba0d915d7e01cfff26b7da6dac9d076e92ffd0965d9724e26b
O=C1OCOC(=O)C1=CNc1ccc(Cc2ccccc2)cc1.O=C1OCOC(=O)C1=CNc1cccc(Cc2ccccc2)c1
[C;D1;H3:1]-[CH2;D2;+0:2]-[O;H0;D2;+0:3]-[CH;D3;+0:4](-[O;H0;D2;+0:5]-[CH2;D2;+0:6]-[CH3;D1;+0:7])-[O;H0;D2;+0:8]-[CH2;D2;+0:9]-[CH3;D1;+0:10].[C;D1;H3:11]-[C:12]1(-[C;D1;H3:13])-[#8:14]-[C:15](=[O;D1;H0:16])-[CH2;D2;+0:17]-[C;H0;D3;+0:18](=[O;D1;H0:19])-[O;H0;D2;+0:20]-1.[NH2;D1;+0:21]-[c:22](:[c:23]):[c:24].[NH2;D1;+...
null
[]
null
null
null
null
Triethyl orthoformate (10.0 mL, 60.1 mmol), Meldrum's acid (8.2 g, 57 mmol), and either 3-benzyl aniline or 4-benzyl aniline (10.0 g, 54.6 mmol) as indicated in the table below in methanol (303 mL) were combined and treated according to the method described in Part A of Example 1 to provide 5-[(3-benzylphenylamino)meth...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Ether.Ether.Ether.Primary amine.Primary amine
Enamine.Enamine.Ester.Ester.Ester.Ester
C1COCOC1
C1COCOC1.C1COCOC1
C1COCOC1.c1ccccc1.c1ccccc1.C1COCOC1.c1ccccc1.c1ccccc1
Other
CO
null
null
CC1(C)OC(=O)CC(=O)O1.CCOC(OCC)OCC.Nc1ccc(Cc2ccccc2)cc1.Nc1cccc(Cc2ccccc2)c1>CO>CC1(C)OC(=O)C(=CNc2ccc(Cc3ccccc3)cc2)C(=O)O1.CC1(C)OC(=O)C(=CNc2cccc(Cc3ccccc3)c2)C(=O)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-784d2dd1f34043149cecc0d483a46e48
O=[N+]([O-])O.Oc1ccnc2cc(Cc3ccccc3)ccc12.Oc1ccnc2ccc(Cc3ccccc3)cc12>>O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1O.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1O
C(C1=CC=CC=C1)C1=CC=C2C(=CC=NC2=C1)O.C(C1=CC=CC=C1)C=1C=C2C(=CC=NC2=CC1)O.[N+](=O)(O)[O-]>>C(C1=CC=CC=C1)C1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])O.C(C1=CC=CC=C1)C=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])O
[O:1]=[N+:23]([OH:3])[O-:24].[cH:4]1[cH:5][n:6][c:7]2[cH:8][c:9]([CH2:10][c:11]3[cH:12][cH:13][cH:14][cH:15][cH:16]3)[cH:17][cH:18][c:19]2[c:20]1[OH:21].[n:2]1[cH:26][cH:25][c:41]([OH:42])[c:40]2[c:28]1[cH:29][cH:30][c:31]([CH2:32][c:33]1[cH:34][cH:35][cH:36][cH:37][cH:38]1)[cH:39]2>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][n:...
O=[N+]([O-])O.Oc1ccnc2cc(Cc3ccccc3)ccc12.Oc1ccnc2ccc(Cc3ccccc3)cc12
O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1O.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1O
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
e4cc7b0e705a045ffe673b7312da26eefcc4ceb4b30b7b809794b816d906d64d
6674cfa36c1a7a9bb1f0df0b4aa5b94d1b581f7b4be96876f34ffacfa3ea15db
c1ccc(Cc2ccc3cccnc3c2)cc1.c1ccc(Cc2ccc3ncccc3c2)cc1
[O;-;D1;H0:1]-[N+;H0;D3:2](=[O;H0;D1;+0:3])-[OH;D1;+0:4].[O;D1;H1:5]-[c:6]1:[cH;D2;+0:7]:[cH;D2;+0:8]:[n;H0;D2;+0:9]:[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:1:[c:14].[O;D1;H1:15]-[c:16]1:[c:17]:[c:18]:[#7;a:19]:[c:20]:[cH;D2;+0:21]:1>>[O-;H0;D1:4]-[N+;H0;D3:9](=[O;H0;D1;+0:3])-[c;H0;D3;+0:21]1:[c:20]:[#7;a:19]:[c:18]:[c...
null
[]
null
null
null
null
The method described in Part D of Example 10 was used to treat 7-benzylquinolin-4-ol or 6-benzylquinolin-4-ol with nitric acid to provide 7-benzyl-3-nitroquinolin-4-ol or 6-benzyl-3-nitroquinolin-4-ol, respectively, as solids. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group.Nitro group
c1ccc2ncccc2c1.c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1.c1ccc2ncccc2c1.c1ccccc1
null
null
null
null
O=[N+]([O-])O.Oc1ccnc2cc(Cc3ccccc3)ccc12.Oc1ccnc2ccc(Cc3ccccc3)cc12>>O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1O.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-89dff75aa83d4c2c8be904ac12f724d0
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1O.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1O>>O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1Cl.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1Cl
C(C1=CC=CC=C1)C1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])O.C(C1=CC=CC=C1)C=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])O.P(=O)(Cl)(Cl)Cl>>C(C1=CC=CC=C1)C1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.C(C1=CC=CC=C1)C=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])Cl
O=P(Cl)([Cl:21])[Cl:42].O[c:20]1[c:4]([N+:2](=[O:1])[O-:3])[cH:5][n:6][c:7]2[cH:8][c:9]([CH2:10][c:11]3[cH:12][cH:13][cH:14][cH:15][cH:16]3)[cH:17][cH:18][c:19]21.O[c:41]1[c:25]([N+:23](=[O:22])[O-:24])[cH:26][n:27][c:28]2[cH:29][cH:30][c:31]([CH2:32][c:33]3[cH:34][cH:35][cH:36][cH:37][cH:38]3)[cH:39][c:40]21>>[O:1]=[N...
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1O.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1O
O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1Cl.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1Cl
null
null
null
Functional Group Addition
OtherReaction
62803afad24e75ce74a549b9c7ab0a60972fe8d8e6a394f7f72b0523bceb62a4
d74bc1b012061488363cc8b67469d047228fe70d9f227566212bf2539e8291df
c1ccc(Cc2ccc3cccnc3c2)cc1.c1ccc(Cc2ccc3ncccc3c2)cc1
Cl-P(=O)(-[Cl;H0;D1;+0:1])-[Cl;H0;D1;+0:2].O-[c;H0;D3;+0:3]1:[c:4](-[#7;+:5]):[c:6]:[#7;a:7]:[c:8](:[c:9]):[c:10]:1:[c:11].O-[c;H0;D3;+0:12]1:[c:13](:[c:14]):[c:15](:[c:16]):[#7;a:17]:[c:18]:[c:19]:1-[#7;+:20]>>[#7;+:20]-[c:19]1:[c:18]:[#7;a:17]:[c:15](:[c:16]):[c:13](:[c:14]):[c;H0;D3;+0:12]:1-[Cl;H0;D1;+0:1].[#7;+:5]...
null
[]
null
null
null
null
The method described in Part E of Example 10 was used to treat 7-benzyl-3-nitroquinolin-4-ol or 6-benzyl-3-nitroquinolin-4-ol with phosphorous oxychloride to provide 7-benzyl-4-chloro-3-nitroquinoline as a light yellow powder or 6-benzyl-4-chloro-3-nitroquinoline as a tan powder, respectively. Conditions: See reaction....
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol.Aromatic alcohol
Aromatic halide.Aromatic halide
c1ccc2ncccc2c1.c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1.c1ccc2ncccc2c1.c1ccccc1
HCl
null
null
null
O=P(Cl)(Cl)Cl.O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1O.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1O>>O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1Cl.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1Cl
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a26247a753df407cb8aa5733bcc350c4
CC(C)(O)CN.CCN(CC)CC.O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1Cl.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1Cl>>CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccc(Cc3ccccc3)cc12
NCC(C)(O)C.C(C1=CC=CC=C1)C1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.C(C1=CC=CC=C1)C=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])Cl.C(C)N(CC)CC>>C(C1=CC=CC=C1)C1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC(C)(O)C.C(C1=CC=CC=C1)C=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])NCC(C)(O)C
[CH3:27][C:28]([CH3:29])([OH:30])[CH2:31][NH2:32].C[CH2:5][N:6](C[CH3:3])[CH2:2][CH3:1].Cl[c:7]1[c:8]([N+:9](=[O:10])[O-:11])[cH:12][n:13][c:14]2[cH:15][c:16]([CH2:17][c:18]3[cH:19][cH:20][cH:21][cH:22][cH:23]3)[cH:24][cH:25][c:26]12.Cl[c:33]1[c:34]([N+:35](=[O:4])[O-:36])[cH:38][n:39][c:40]2[cH:41][cH:42][c:43]([CH2:4...
CC(C)(O)CN.CCN(CC)CC.O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1Cl.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1Cl
CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccc(Cc3ccccc3)cc12
null
null
ClCCl
Heteroatom Alkylation and Arylation
OtherReaction
8070e49a703ee32ad1c4b70cc94cc74c320661b4caef4617a6bf3fecf414c14f
545f73d1df2c6f4b6586383103a73876f5ba179ddc71535c47c7b1c16ee04be1
c1ccc(Cc2ccc3cccnc3c2)cc1.c1ccc(Cc2ccc3ncccc3c2)cc1
C-[CH2;D2;+0:1]-[N;H0;D3;+0:2](-C-[CH3;D1;+0:3])-[CH2;D2;+0:4]-[C;D1;H3:5].Cl-[c;H0;D3;+0:6]1:[c:7](-[N+;H0;D3:8](-[O-;H0;D1:9])=[O;H0;D1;+0:10]):[c:11]:[#7;a:12]:[c:13](:[c:14]):[c:15]:1:[c:16].Cl-[c;H0;D3;+0:17]1:[c:18](:[c:19]):[c:20](:[c:21]):[#7;a:22]:[c:23]:[c:24]:1-[#7;+:25].[C:26]-[C:27]-[NH2;D1;+0:28]>>[#7;+:2...
null
[]
null
null
8
HOUR
Under a nitrogen atmosphere, 1-amino-2-methylpropan-2-ol (1.2 equivalents) was added to a 0.2 M solution of 7-benzyl-4-chloro-3-nitroquinoline or 6-benzyl-4-chloro-3-nitroquinoline (1 equivalent) and triethylamine (3 equivalents) in dichloromethane, and the reaction was stirred overnight at ambient temperature. The vol...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Nitro group.Primary amine.Tertiary amine
Nitro group.Tertiary alcohol.Secondary amine.Secondary amine
c1ccc2ncccc2c1.c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccccc1.c1ccc2ncccc2c1.c1ccccc1
HCl
ClCCl
null
8
CC(C)(O)CN.CCN(CC)CC.O=[N+]([O-])c1cnc2cc(Cc3ccccc3)ccc2c1Cl.O=[N+]([O-])c1cnc2ccc(Cc3ccccc3)cc2c1Cl>ClCCl>CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccc(Cc3ccccc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8dca345f64d74c3baa164565dcda69f8
CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccc(Cc3ccccc3)cc12>>CC(C)(O)CNc1c(N)cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c(N)cnc2ccc(Cc3ccccc3)cc12
C(C1=CC=CC=C1)C1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC(C)(O)C.C(C1=CC=CC=C1)C=1C=C2C(=C(C=NC2=CC1)[N+](=O)[O-])NCC(C)(O)C>>NC=1C=NC2=CC(=CC=C2C1NCC(C)(O)C)CC1=CC=CC=C1.NC=1C=NC2=CC=C(C=C2C1NCC(C)(O)C)CC1=CC=CC=C1
O=[N+:9]([O-])[c:8]1[c:7]([NH:6][CH2:5][C:2]([CH3:1])([CH3:3])[OH:4])[c:24]2[c:12]([n:11][cH:10]1)[cH:13][c:14]([CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1)[cH:22][cH:23]2.O=[N+:33]([O-])[c:32]1[c:31]([NH:30][CH2:29][C:26]([CH3:25])([CH3:27])[OH:28])[c:48]2[c:36]([n:35][cH:34]1)[cH:37][cH:38][c:39]([CH2:40][c:4...
CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccc(Cc3ccccc3)cc12
CC(C)(O)CNc1c(N)cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c(N)cnc2ccc(Cc3ccccc3)cc12
null
null
null
Functional Group Interconversion
OtherReaction
f469aaae1e88945b257afa41cebe21597b9a3f326d9f2ab1d5670c64dd831541
86e032c8ebc9cbcd13a880d0d66c541ff63611af16d12657aad958d17abf4587
c1ccc(Cc2ccc3cccnc3c2)cc1.c1ccc(Cc2ccc3ncccc3c2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].O=[N+;H0;D3:7](-[O-])-[c:8](:[c:9]):[c:10]:[#7;a:11]:[c:12]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[NH2;D1;+0:7]-[c:8](:[c:9]):[c:10]:[#7;a:11]:[c:12]
null
[]
null
null
2
DAY
A modification of the method described in Part A of Examples 427–429 was used to reduce 1-(7-benzyl-3-nitroquinolin-4-ylamino)-2-methylpropan-2-ol or 1-(6-benzyl-3-nitroquinolin-4-ylamino)-2-methylpropan-2-ol. The reaction was shaken for one or two days to provide 1-(3-amino-7-benzylquinolin-4-ylamino)-2-methylpropan-2...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Nitro group
Primary amine.Primary amine
null
null
c1ccc2ncccc2c1.c1ccccc1.c1ccc2ncccc2c1.c1ccccc1
Other
null
null
48
CC(C)(O)CNc1c([N+](=O)[O-])cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c([N+](=O)[O-])cnc2ccc(Cc3ccccc3)cc12>>CC(C)(O)CNc1c(N)cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c(N)cnc2ccc(Cc3ccccc3)cc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7c4ba5b0737a4f89b2ca5ce53f1a44b3
CC(C)(O)CNc1c(N)cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c(N)cnc2ccc(Cc3ccccc3)cc12>>CC(C)(O)Cn1cnc2cnc3cc(Cc4ccccc4)ccc3c21.CC(C)(O)Cn1cnc2cnc3ccc(Cc4ccccc4)cc3c21
NC=1C=NC2=CC(=CC=C2C1NCC(C)(O)C)CC1=CC=CC=C1.NC=1C=NC2=CC=C(C=C2C1NCC(C)(O)C)CC1=CC=CC=C1.C(OCC)(OCC)OCC>>C(C1=CC=CC=C1)C=1C=CC=2C3=C(C=NC2C1)N=CN3CC(C)(O)C.C(C1=CC=CC=C1)C1=CC=2C3=C(C=NC2C=C1)N=CN3CC(C)(O)C
[CH3:1][C:2]([CH3:3])([OH:4])[CH2:5][NH:6][c:25]1[c:9]([NH2:8])[cH:10][n:11][c:12]2[cH:13][c:14]([CH2:15][c:16]3[cH:17][cH:18][cH:19][cH:20][cH:21]3)[cH:22][cH:23][c:24]21.[CH3:26][C:27]([CH3:28])([OH:29])[CH2:30][NH:31][c:50]1[c:34]([NH2:33])[cH:35][n:36][c:37]2[cH:38][cH:39][c:40]([CH2:41][c:42]3[cH:43][cH:44][cH:45]...
CC(C)(O)CNc1c(N)cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c(N)cnc2ccc(Cc3ccccc3)cc12
CC(C)(O)Cn1cnc2cnc3cc(Cc4ccccc4)ccc3c21.CC(C)(O)Cn1cnc2cnc3ccc(Cc4ccccc4)cc3c21
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b6eba0d3ddf07d65a738d182c49e05e581b7c331dc24811a5939a71fcbc7ae87
23443a0287b53d223fe3b7fe1486262eb4d997ce605d04f578cd81fe2405710e
c1ccc(Cc2ccc3c(c2)ncc2nc[nH]c23)cc1.c1ccc(Cc2ccc3ncc4nc[nH]c4c3c2)cc1
[C:1]-[C:2]-[NH;D2;+0:3]-[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1-[NH2;D1;+0:10].[C:11]-[C:12]-[NH;D2;+0:13]-[c:14]1:[c:15]:[c:16]:[#7;a:17]:[c:18]:[c:19]:1-[NH2;D1;+0:20]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[c:21]:[n;H0;D2;+0:10]:[c:9]2:[c:8]:[#7;a:7]:[c:6]:[c:5]:[c:4]:2:1.[C:11]-[C:12]-[n;H0;D3;+0:13]1:[c:22]:[n;H0;D2;+0:2...
null
[]
null
null
8
HOUR
For Examples 431 and 434, a modification of the method described in Part B of Examples 427–429 was used to treat 1-(3-amino-7-benzylquinolin-4-ylamino)-2-methylpropan-2-ol or 1-(3-amino-6-benzylquinolin-4-ylamino)-2-methylpropan-2-ol with triethyl orthoformate, as indicated in the table below. The reaction was heated a...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Primary amine.Secondary amine.Secondary amine
null
c1ccc2ncccc2c1.c1ccc2ncccc2c1
c1ccc2c(c1)ncc1nc[nH]c12.c1ccc2ncc3nc[nH]c3c2c1
c1ccc2c(c1)ncc1nc[nH]c12.c1ccccc1.c1ccc2ncc3nc[nH]c3c2c1.c1ccccc1
Other
null
null
8
CC(C)(O)CNc1c(N)cnc2cc(Cc3ccccc3)ccc12.CC(C)(O)CNc1c(N)cnc2ccc(Cc3ccccc3)cc12>>CC(C)(O)Cn1cnc2cnc3cc(Cc4ccccc4)ccc3c21.CC(C)(O)Cn1cnc2cnc3ccc(Cc4ccccc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-87647dbc841a4245be527a11092613db
NCC1CCCCC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCC1CCCCC1
C1(CCCCC1)CN.BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC1CCCCC1
[NH2:15][CH2:16][CH:17]1[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]1.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][CH:17]1[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]1
NCC1CCCCC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCC1CCCCC1
null
null
ClCCl
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2c(NCC3CCCCC3)ccnc2c1
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]
62.8
[{"value": 62.8, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC1CCCCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
Under a nitrogen atmosphere, cyclohexylmethylamine (40.9 mL, 315 mmol) was added dropwise to a solution of 7-bromo-4-chloro-3-nitroquinoline (30.0 g, 105 mmol) in dichloromethane (524 mL). The reaction was stirred for 18 hours at ambient temperature and then concentrated under reduced pressure. Water (200 mL) was added...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.C1CCCCC1
HCl
ClCCl
null
18
NCC1CCCCC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>ClCCl>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCC1CCCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f41eaa09f57b47d7a510a6dea1c16c23
CCOCC(=O)Cl.Nc1cnc2cc(Br)ccc2c1NCC1CCCCC1>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCCCC1
BrC1=CC=C2C(=C(C=NC2=C1)N)NCC1CCCCC1.C(C)OCC(=O)Cl>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC3CCCCC3)COCC
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]([Br:13])[cH:14][cH:15][c:16]2[c:17]1[NH:18][CH2:19][CH:20]1[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]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]1[...
CCOCC(=O)Cl.Nc1cnc2cc(Br)ccc2c1NCC1CCCCC1
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCCCC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
101a087a520f159c722ba3d78ed38f5c3c1cf154206e5edbeb1e6397c929560f
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
c1ccc2c(c1)ncc1ncn(CC3CCCCC3)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]
null
[]
90
CELSIUS
null
null
A modification of the method described in Part A of Example 9 was used to treat 7-bromo-N4-(cyclohexylmethyl)quinoline-3,4-diamine (7.3 g, 22 mmol) with ethoxyacetyl chloride (2.75 mL, 24.0 mmol). The reaction was heated overnight at 90° C. and then concentrated under reduced pressure to provide 7-bromo-1-cylcohexylmet...
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
HCl
null
90
null
CCOCC(=O)Cl.Nc1cnc2cc(Br)ccc2c1NCC1CCCCC1>>CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5c4046931f764f058fe2c1ac6ff47cc0
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCCCC1.[NH4+]>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCCCC1
BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC3CCCCC3)COCC.ClC=1C=C(C(=O)OO)C=CC1.[OH-].[NH4+].C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC3CCCCC3)COCC
[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][CH:21]1[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]1.[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:17]3[c:18]2[n:19]1[CH2:2...
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCCCC1.[NH4+]
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCCCC1
null
null
C(C)#N
Functional Group Addition
OtherReaction
dc63235befaaf41df35292b6862b726098d8e1b79a2cef881f35b7cf9ff16606
d69ce1fde4173969963123914389bef807fad83b73b8a587195a7122d5cdf1d2
c1ccc2c(c1)ncc1ncn(CC3CCCCC3)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
null
null
The method described in Part J of Example 365 was used to oxidize and aminate 7-bromo-1-cylcohexylmethyl-2-ethoxymethyl-1H-imidazo[4,5-c]quinoline (7.58 g, 22.0 mmol). 3-Chloroperoxybenzoic acid (9.1 g of 50% pure material, 26.4 mmol) was added in five portions during the oxidation step, and the amination with ammonium...
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.C1CCCCC1
null
C(C)#N
null
null
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCCCC1.[NH4+]>C(C)#N>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-796b06cb40f64989bb91238e51ff606a
CC(C)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>CC(C)CNc1c(N)cnc2cc(Br)ccc12
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
[Pt]
C1(=CC=CC=C1)C
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]
null
[]
null
null
8
HOUR
(7-Bromo-3-nitroquinolin-4-yl)-(2-methylpropyl)amine (117 g) was dissolved in hot toluene (2 L) and poured into stainless steel Parr vessel. Additional toluene (2 L) and 5% platinum on carbon (12.5 g) were added. The vessel was evacuated, charged with hydrogen (54 psi, 3.7×105 Pa), and shaken overnight at room temperat...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C1(=CC=CC=C1)C
null
8
CC(C)CNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>[Pt].C1(=CC=CC=C1)C>CC(C)CNc1c(N)cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e8cfcc7d7bdb4706b163b70ba212038d
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCCC(=O)Cl>>CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
C(CCC)(=O)Cl.BrC1=CC=C2C(=C(C=NC2=C1)N)NCC(C)C>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)C)CCC
[NH2:5][c:6]1[cH:7][n:8][c:9]2[cH:10][c:11]([Br:12])[cH:13][cH:14][c:15]2[c:16]1[NH:17][CH2:18][CH:19]([CH3:20])[CH3:21].O=[C:4](Cl)[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]([Br:12])[cH:13][cH:14][c:15]3[c:16]2[n:17]1[CH2:18][CH:19]([CH3:20])[CH3:21]
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCCC(=O)Cl
CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
null
[Au]
N1=CC=CC=C1
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]
null
[]
null
null
null
null
Butyryl chloride (1.1 equivalent) was slowly added to a stirred solution of 7-bromo-N4-(2-methylpropyl)quinoline-3,4-diamine (52.9 g, 0.18 mol.) in pyridine (700 mL) at room temperature. A pale yellow precipitate formed and then went into solution. The reaction mixture was heated at reflux for eight hours, and then all...
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
[Au].N1=CC=CC=C1
null
null
CC(C)CNc1c(N)cnc2cc(Br)ccc12.CCCC(=O)Cl>[Au].N1=CC=CC=C1>CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-27bcffb2956c4abb8cb2439f0cab4e5f
CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C.[NH4+]>>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C
C1(=CC=C(C=C1)S(=O)(=O)Cl)C.BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC(C)C)CCC.ClC=1C=C(C(=O)OO)C=CC1.[OH-].[NH4+]>>BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCC
[CH3:1][CH2:2][CH2:3][c:4]1[n:5][c:6]2[cH:7][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].[NH4+:8]>>[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]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH:20]([CH3:21])[CH3:22]
CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C.[NH4+]
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C
null
null
ClCCl
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
15
MINUTE
To a stirred solution of 7-bromo-1-(2-methylpropyl)-2-propyl-1H-imidazo[4,5-c]quinoline (51.1 g, 0.148 mol) in dichloromethane (1 L) was slowly added 3-chloroperoxybenzoic acid (1.0 equivalent of 50% pure material) in small portions. The reaction was maintained at room temperature for one hour. Concentrated ammonium hy...
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
null
0.25
CCCc1nc2cnc3cc(Br)ccc3c2n1CC(C)C.[NH4+]>ClCCl>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f3deeef20851413a8d51142d4d2c4924
C=C[B-](F)(F)F.CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C>>C=Cc1ccc2c(c1)nc(N)c1nc(CCC)n(CC(C)C)c12
C(C)N(CC)CC.C(=C)[B-](F)(F)F.[K+].BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)C)CCC.[OH-].[Na+]>>CC(CN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=C)N)CCC)C
F[B-](F)(F)[CH:2]=[CH2:1].Br[c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[n:9][c:10]([NH2:11])[c:12]1[n:13][c:14]([CH2:15][CH2:16][CH3:17])[n:18]([CH2:19][CH:20]([CH3:21])[CH3:22])[c:23]21>>[CH2:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[n:9][c:10]([NH2:11])[c:12]1[n:13][c:14]([CH2:15][CH2:16][CH3:17])[n:18]([CH2:19][CH:...
C=C[B-](F)(F)F.CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C
C=Cc1ccc2c(c1)nc(N)c1nc(CCC)n(CC(C)C)c12
null
C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2]
C(CC)O.O
Functional Group Interconversion
OtherReaction
b6174e4193e02027d22a36dfa7ee1eca16a8f84c44e86ec780137145ed7eacc0
493c526dad91fdaab0a79ca6b28939f7e66256ca7a9e4efc8dfd07eebbd72256
c1ccc2c(c1)ncc1nc[nH]c12
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]2:[c:5](:[#7;a:6]):[c:7](:[#7;a:8]):[c:9]:[#7;a:10]:[c:11]:2:[c:12]:1.F-[B-](-F)(-F)-[CH;D2;+0:13]=[C;D1;H2:14]>>[#7;a:8]:[c:7]1:[c:9]:[#7;a:10]:[c:11]2:[c:12]:[c;H0;D3;+0:1](-[CH;D2;+0:13]=[C;D1;H2:14]):[c:2]:[c:3]:[c:4]:2:[c:5]:1:[#7;a:6]
null
[]
null
null
null
null
Triethylamine (3.0 equivalents), potassium vinyltrifluoroborate (1.0 equivalent) and dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium (II) dichloromethane adduct (0.2 equivalent) were added to a solution of 7-bromo-1-(2-methylpropyl)-2-propyl-1H-imidazo[4,5-c]quinolin-4-amine (1.0 equivalent) in n-propanol (30 m...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Vinyl
Vinyl
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
Br-.B
C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].C(CC)O.O
null
null
C=C[B-](F)(F)F.CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)C>C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].C(CC)O.O>C=Cc1ccc2c(c1)nc(N)c1nc(CCC)n(CC(C)C)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a0b7a3a3e0674a5c922c7e18e8da34dc
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCOC.c1cn[nH]c1>>CCOCc1nc2c(N)nc3cc(-n4cccn4)ccc3c2n1CCCOC
P(=O)([O-])([O-])[O-].[K+].[K+].[K+].N1N=CC=C1.BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CCCOC)COCC.N[C@H]1[C@@H](CCCC1)N>>C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)N2N=CC=C2)N)N1)CCCOC
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][CH2:25][CH2:26][O:27][CH3:28])[c:22]3[c:21]2[cH:20][cH:19]1.[nH:14]1[cH:15][cH:16][cH:17][n: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](-[n:14]4[cH:15][cH:16][cH:17][n:18]...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCOC.c1cn[nH]c1
CCOCc1nc2c(N)nc3cc(-n4cccn4)ccc3c2n1CCCOC
null
[Cu]I
O1CCOCC1
Heteroatom Alkylation and Arylation
OtherReaction
34efca80a73526f58805156846e0cfaa34d4d87fbfddf09fd49bf5f9e2f9ed6b
e3660767655c50df0f92afc78c794dd2af7cf646bf1430960eafd30c23bf3fa7
c1cnn(-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.[#7;a:13]1:[c:14]:[c:15]:[c:16]:[nH;D2;+0:17]:1>>[#7;a:9]:[c:8]1:[c:10]2:[c:11]:[c:12]:[c;H0;D3;+0:1](-[n;H0;D3;+0:17]3:[#7;a:13]:[c:14]:[c:15]:[c:16]:3):[c:2]:[c:3]:2:[#7;a:4]:[c:5]:[c:6]:1:[#7;a:7]
25
[{"value": 25.0, "product": "C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)N2N=CC=C2)N)N1)CCCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15.5
HOUR
A 4 dram vial containing a stir bar was charged sequentially with copper(I) iodide (0.038 g), potassium phosphate (0.890 g), pyrazole (0.164 g), 7-bromo-2-ethoxymethyl-1-(3-methoxypropyl)-1H-imidazo[4,5-c]quinolin-4-amine (0.786 g), (±)-trans-1,2-diaminocyclohexane (0.030 mL), and anhydrous 1,4-dioxane (2 mL). The vial...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ccc2c(c1)ncc1[nH]cnc12.c1cn[nH]c1
c1ccc2c(c1)ncc1[nH]cnc12.c1cn[nH]c1
c1ccc2c(c1)ncc1[nH]cnc12.c1cn[nH]c1
HBr
[Cu]I.O1CCOCC1
null
15.5
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCOC.c1cn[nH]c1>[Cu]I.O1CCOCC1>CCOCc1nc2c(N)nc3cc(-n4cccn4)ccc3c2n1CCCOC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5574c035cb5d4caf8df4dacdca15baab
COC(=O)C1CCOCC1.[NH4+]>>NC(=O)C1CCOCC1
[OH-].[NH4+].O1CCC(CC1)C(=O)OC.[OH-].[NH4+]>>O1CCC(CC1)C(=O)N
CO[C:2](=[O:3])[CH:4]1[CH2:5][CH2:6][O:7][CH2:8][CH2:9]1.[NH4+:1]>>[NH2:1][C:2](=[O:3])[CH:4]1[CH2:5][CH2:6][O:7][CH2:8][CH2:9]1
COC(=O)C1CCOCC1.[NH4+]
NC(=O)C1CCOCC1
null
null
CO
Acylation
OtherReaction
d5b10d4f469e7a196a3b04a6a9e159a7d90514b6df5b50c1197d4b1b774c04e1
adc0ef6f6c1340dd2dbab737c85bf17fc842769181c5db1a2b4f82b391b28f9f
C1CCOCC1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5].[NH4+;D0:6]>>[C:4]-[C:3](-[C;H0;D3;+0:1](-[NH2;D1;+0:6])=[O;D1;H0:2])-[C:5]
null
[]
null
null
8
HOUR
Ammonium hydroxide (1 L) was added to a solution of methyl tetrahydro-2H-pyran-4-carboxylate (20 mL, 150 mmol) in methanol (500 mL), and the reaction was stirred overnight at ambient temperature. Additional ammonium hydroxide (500 mL) was added, and the reaction was stirred for four additional days. The methanol was re...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary amide
null
null
C1CCOCC1
HO-
CO
null
8
COC(=O)C1CCOCC1.[NH4+]>CO>NC(=O)C1CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f146f725e49749349a288d4b0e2fcd92
NCC1CCOCC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCC1CCOCC1
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.O1CCC(CC1)CN>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC1CCOCC1
[NH2:15][CH2:16][CH:17]1[CH2:18][CH2:19][O:20][CH2:21][CH2:22]1.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][CH:17]1[CH2:18][CH2:19][O:20][CH2:21][CH2:22]1
NCC1CCOCC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCC1CCOCC1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2c(NCC3CCOCC3)ccnc2c1
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]
94.3
[{"value": 94.3, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCC1CCOCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The method described in Part E of Examples 431–436 was used to treat 7-bromo-4-chloro-3-nitroquinoline (12.43 g, 43.45 mmol) with C-(tetrahydropyran-4-yl)methylamine (10 g, 87 mmol) to provide 15.0 g of (7-bromo-3-nitroquinolin-4-yl)(tetrahydropyran-4-ylmethyl)amine as a bright yellow solid. Conditions: See reaction.no...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1.C1CCOCC1
HCl
null
null
null
NCC1CCOCC1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>O=[N+]([O-])c1cnc2cc(Br)ccc2c1NCC1CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-eb25d8f7ee804c1381c56c9177ce0ca8
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCOCC1.[NH4+]>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCOCC1
BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CC3CCOCC3)COCC.ClC=1C=C(C(=O)OO)C=CC1.[OH-].[NH4+].C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC3CCOCC3)COCC
[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][CH:21]1[CH2:22][CH2:23][O:24][CH2:25][CH2:26]1.[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:17]3[c:18]2[n:19]1[CH2:20]...
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCOCC1.[NH4+]
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCOCC1
null
ClC=1C=C(C(=O)OO)C=CC1
C(C)#N
Functional Group Addition
OtherReaction
dc63235befaaf41df35292b6862b726098d8e1b79a2cef881f35b7cf9ff16606
d69ce1fde4173969963123914389bef807fad83b73b8a587195a7122d5cdf1d2
c1ccc2c(c1)ncc1ncn(CC3CCOCC3)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
8
HOUR
The method described in Part J of Example 365 was used to oxidize and aminate 7-bromo-2-ethoxymethyl-1-(tetrahydropyran-4-ylmethyl)-1H-imidazo[4,5-c]quinoline (9.3 g, 23.0 mmol). 3-Chloroperoxybenzoic acid (7.9 g of 50% pure material, 23 mmol) was added in five portions during the oxidation step, which was stirred over...
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.C1CCOCC1
null
ClC=1C=C(C(=O)OO)C=CC1.C(C)#N
null
8
CCOCc1nc2cnc3cc(Br)ccc3c2n1CC1CCOCC1.[NH4+]>ClC=1C=C(C(=O)OO)C=CC1.C(C)#N>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-364907e077a64b9c904a0cc083c30353
CC(C)Cn1cnc2c(N)nc3ccccc3c21.O=[N+]([O-])O>>CC(C)Cn1cnc2c(N)nc3ccc([N+](=O)[O-])cc3c21
[OH-].[NH4+].CC(CN1C=NC=2C(=NC=3C=CC=CC3C21)N)C.[N+](=O)(O)[O-]>>CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)[N+](=O)[O-])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][cH:15][cH:19][c:20]3[c:21]12.O[N+:16](=[O:17])[O-:18]>>[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]([N+:16](=[O:17])[O-:18])[cH:19][c:20]3[c:21]12
CC(C)Cn1cnc2c(N)nc3ccccc3c21.O=[N+]([O-])O
CC(C)Cn1cnc2c(N)nc3ccc([N+](=O)[O-])cc3c21
null
null
S(O)(O)(=O)=O
Functional Group Addition
Aromatic nitration with HNO3
e5a0830ab7d7f820529ff7c5fca2a3f84f966182dcfb90bb0e8e19b90af481f5
ddce49825c02b8965f10c8d99e3c841d26e1f136da6037b417c09313e6d73097
c1ccc2c(c1)ncc1nc[nH]c12
O-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3].[#7;a:4]:[c:5]1:[c:6]:[c:7]:[cH;D2;+0:8]:[c:9]:[c:10]:1:[c:11]:[#7;a:12]>>[#7;a:4]:[c:5]1:[c:6]:[c:7]:[c;H0;D3;+0:8](-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3]):[c:9]:[c:10]:1:[c:11]:[#7;a:12]
null
[]
null
null
2
HOUR
A solution of 1-(2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine (28.3 g, 0.118 mol) in concentrated sulfuric acid (150 mL) was cooled to 5° C. A solution of 70% nitric acid (8.4 mL, 0.130 mol) in sulfuric acid (30 mL) was added in portions over a period of one hour. The reaction temperature was maintained below 10° ...
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group
c1nc2ccccc2c2[nH]cnc12
c1ccc2ncc3nc[nH]c3c2c1
c1ccc2ncc3nc[nH]c3c2c1
HO-
S(O)(O)(=O)=O
null
2
CC(C)Cn1cnc2c(N)nc3ccccc3c21.O=[N+]([O-])O>S(O)(O)(=O)=O>CC(C)Cn1cnc2c(N)nc3ccc([N+](=O)[O-])cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bdb211b4df684f309f1596fd2503ee77
CC(C)Cn1cnc2c(N)nc3ccc(N)cc3c21.COC1CCC(OC)O1>>CC(C)Cn1cnc2c(N)nc3ccc(-n4cccc4)cc3c21
COC1OC(CC1)OC.NC1=CC=2C3=C(C(=NC2C=C1)N)N=CN3CC(C)C>>CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)N2C=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]([NH2:16])[cH:21][c:22]3[c:23]12.CO[CH:17]1O[CH:20](OC)[CH2:19][CH2:18]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](-[n:16]4[cH:17][cH:18][cH:19][cH:20]4)[cH:21]...
CC(C)Cn1cnc2c(N)nc3ccc(N)cc3c21.COC1CCC(OC)O1
CC(C)Cn1cnc2c(N)nc3ccc(-n4cccc4)cc3c21
null
null
C(C)(=O)O
Aromatic Heterocycle Formation
OtherReaction
0e9d22b0723ec2930c6f0b28cb06c2d86835df697b962917265b2a52889a76e9
37da407ba22aeb87f9320448e7710117027e549cd7c89e722598c54789c5481f
c1ccn(-c2ccc3ncc4nc[nH]c4c3c2)c1
C-O-[CH;D3;+0:1]1-O-[CH;D3;+0:2](-O-C)-[CH2;D2;+0:3]-[CH2;D2;+0:4]-1.[#7;a:5]:[c:6]1:[c:7]:[c:8]:[c;H0;D3;+0:9](-[NH2;D1;+0:10]):[c:11]:[c:12]:1:[c:13]:[#7;a:14]>>[#7;a:5]:[c:6]1:[c:7]:[c:8]:[c;H0;D3;+0:9](-[n;H0;D3;+0:10]2:[cH;D2;+0:1]:[cH;D2;+0:4]:[cH;D2;+0:3]:[cH;D2;+0:2]:2):[c:11]:[c:12]:1:[c:13]:[#7;a:14]
57.3
[{"value": 57.3, "product": "CC(CN1C=NC=2C(=NC=3C=CC(=CC3C21)N2C=CC=C2)N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
2,5-Dimethoxytetrahydrofuran (1.6 mL of 95%, 12 mmol) was added to a suspension of 8-amino-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine (3.0 g, 12 mmol) in acetic acid (60 mL), and the reaction was heated at reflux for one hour. The resulting dark brown solution was concentrated under reduced pressure, and the ...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine
null
C1CCOC1
c1cc[nH]c1
c1ccc2ncc3nc[nH]c3c2c1.c1cc[nH]c1
HO-
C(C)(=O)O
null
0.5
CC(C)Cn1cnc2c(N)nc3ccc(N)cc3c21.COC1CCC(OC)O1>C(C)(=O)O>CC(C)Cn1cnc2c(N)nc3ccc(-n4cccc4)cc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b1f865ef25a04e39839832f0be237929
CC1(C)OC(=O)C(=CNc2cccc(Br)c2)C(=O)O1>>Oc1ccnc2cc(Br)ccc12.Oc1ccnc2cccc(Br)c12
BrC=1C=C(C=CC1)NC=C1C(OC(OC1=O)(C)C)=O>>BrC1=CC=C2C(=CC=NC2=C1)O.BrC1=C2C(=CC=NC2=CC=C1)O
O=[C:18]1O[C:14]([CH3:15])([CH3:20])[O:13][C:2](=[O:1])[C:3]1=[CH:4][NH:5][c:6]1[cH:7][c:8]([Br:9])[cH:10][cH:11][cH:12]1>>[OH:1][c:2]1[cH:3][cH:4][n:5][c:6]2[cH:7][c:8]([Br:9])[cH:10][cH:11][c:12]12.[OH:13][c:14]1[cH:15][cH:16][n:17][c:18]2[cH:19][cH:20][cH:21][c:22]([Br:23])[c:24]12
CC1(C)OC(=O)C(=CNc2cccc(Br)c2)C(=O)O1
Oc1ccnc2cc(Br)ccc12.Oc1ccnc2cccc(Br)c12
null
null
C1=CC=C(C=C1)C2=CC=CC=C2.C1=CC=C(C=C1)OC2=CC=CC=C2
Aromatic Heterocycle Formation
OtherReaction
5f75dae222d74bb9fc2b294b367403a07bdf8272477d1afc70174e15b1e90f5d
c37506458ef2b9e2def05ab89db5b266098a3ec74f2476e997b750208146ef63
c1ccc2ncccc2c1.c1ccc2ncccc2c1
O=[C;H0;D3;+0:1]1-O-[C;H0;D4;+0:2](-[CH3;D1;+0:3])(-[CH3;D1;+0:4])-[O;H0;D2;+0:5]-[C;H0;D3;+0:6](=[O;H0;D1;+0:7])-[C;H0;D3;+0:8]-1=[CH;D2;+0:9]-[NH;D2;+0:10]-[c:11](:[c:12]):[cH;D2;+0:13]:[c:14]:[c:15]>>[OH;D1;+0:7]-[c;H0;D3;+0:6]1:[cH;D2;+0:8]:[cH;D2;+0:9]:[n;H0;D2;+0:10]:[c:11](:[c:12]):[c;H0;D3;+0:13]:1:[c:14]:[c:15...
null
[]
null
null
null
null
5-[(3-Bromophenylamino)methylene]-2,2-dimethyl-[1,3]dioxane-4,6-dione (32.6 g, 0.100 mol) was heated at 250° C. in DOWTHERM A heat transfer fluid for one hour, and then the reaction was allowed to cool to ambient temperature. A precipitate formed upon cooling and was isolated by filtration and washed with diethyl ether...
10.6084/m9.figshare.5104873.v1
null
Enamine.Ester.Ester
Aromatic halide.Aromatic alcohol.Aromatic alcohol
C1COCOC1.c1ccccc1
c1ccc2ncccc2c1.c1ccc2ncccc2c1
c1ccc2ncccc2c1.c1ccc2ncccc2c1
null
C1=CC=C(C=C1)C2=CC=CC=C2.C1=CC=C(C=C1)OC2=CC=CC=C2
null
null
CC1(C)OC(=O)C(=CNc2cccc(Br)c2)C(=O)O1>C1=CC=C(C=C1)C2=CC=CC=C2.C1=CC=C(C=C1)OC2=CC=CC=C2>Oc1ccnc2cc(Br)ccc12.Oc1ccnc2cccc(Br)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-85819ad6c6834adb8e5accf545355994
CC(C)CNc1c(N)cnc2cccc(Br)c12>>CC(C)Cn1cnc2cnc3cccc(Br)c3c21
BrC1=C2C(=C(C=NC2=CC=C1)N)NCC(C)C.C(OCC)(OCC)OCC.Cl.N1=CC=CC=C1>>BrC=1C=2C3=C(C=NC2C=CC1)N=CN3CC(C)C
[CH3:1][CH:2]([CH3:3])[CH2:4][NH:5][c:18]1[c:8]([NH2:7])[cH:9][n:10][c:11]2[cH:12][cH:13][cH:14][c:15]([Br:16])[c:17]21>>[CH3:1][CH:2]([CH3:3])[CH2:4][n:5]1[cH:6][n:7][c:8]2[cH:9][n:10][c:11]3[cH:12][cH:13][cH:14][c:15]([Br:16])[c:17]3[c:18]12
CC(C)CNc1c(N)cnc2cccc(Br)c12
CC(C)Cn1cnc2cnc3cccc(Br)c3c21
null
null
C(C)#N
Aromatic Heterocycle Formation
OtherReaction
eb766b33cc37973e90b0a06e1adfb35c78d598e09189e9099c509c7d0e4a7793
c12bf4e666f812d0e692aca3756678364265d1c8b3469e9563c84f9ed1df94d2
c1ccc2c(c1)ncc1nc[nH]c12
[C:1]-[C:2]-[NH;D2;+0:3]-[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1-[NH2;D1;+0:10]>>[C:1]-[C:2]-[n;H0;D3;+0:3]1:[c:11]:[n;H0;D2;+0:10]:[c:9]2:[c:8]:[#7;a:7]:[c:6]:[c:5]:[c:4]:2:1
null
[]
null
null
null
null
A mixture of 5-bromo-N4-(2-methylpropyl)quinoline-3,4-diamine (1.0 g, 3.4 mmol), triethyl orthoformate (0.9 mL, 5 mmol), and pyridine hydrochloride (117 mg, 1.0 mmol) in acetonitrile (17 mL) was heated at reflux overnight. The reaction mixture was concentrated under reduced pressure, and the residue was purified by HPF...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1cccc2ncc3nc[nH]c3c12
c1cccc2ncc3nc[nH]c3c12
Other
C(C)#N
null
null
CC(C)CNc1c(N)cnc2cccc(Br)c12>C(C)#N>CC(C)Cn1cnc2cnc3cccc(Br)c3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b7318fcfda094b7d96708957c22d1daf
CC(C)Cn1cnc2cnc3cccc(Br)c3c21.OB(O)c1ccccc1>>CC(C)Cn1cnc2cnc3cccc(-c4ccccc4)c3c21
BrC=1C=2C3=C(C=NC2C=CC1)N=CN3CC(C)C.C1(=CC=CC=C1)B(O)O>>CC(CN1C=NC=2C=NC=3C=CC=C(C3C21)C2=CC=CC=C2)C
Br[c:15]1[cH:14][cH:13][cH:12][c:11]2[n:10][cH:9][c:8]3[n:7][cH:6][n:5]([CH2:4][CH:2]([CH3:1])[CH3:3])[c:23]3[c:22]21.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[cH:9][n:10][c:11]3[cH:12][cH:13][cH:14][c:15](-[c:16]4[cH:17][cH:18][cH:19][cH:20][cH:21]4)[c:22]3[...
CC(C)Cn1cnc2cnc3cccc(Br)c3c21.OB(O)c1ccccc1
CC(C)Cn1cnc2cnc3cccc(-c4ccccc4)c3c21
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
4ccbd71978726c37809efbeb35dc94765cb7edf530e87f54e6de7a8542442ba8
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cccc3ncc4nc[nH]c4c23)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[c:5]2:[#7;a:6]:[c:7]:[c:8]3:[#7;a:9]:[c:10]:[#7;a:11](-[C:12]):[c:13]:3:[c:14]:2:1.O-B(-O)-[c;H0;D3;+0:15](:[c:16]:[c:17]):[c:18]:[c:19]>>[C:12]-[#7;a:11]1:[c:10]:[#7;a:9]:[c:8]2:[c:7]:[#7;a:6]:[c:5]3:[c:4]:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:15](:[c:16]:[c:17]):[c:18]:[c:19]):...
null
[]
null
null
null
null
9-Bromo-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinoline (0.34 mmol) and benzene boronic acid (62 mg, 0.51 mmol) were coupled according to Part J of Example 1. The work-up procedure described in Parts 125–135 was followed. The crude product was purified by HPFC (eluting with chloroform:CMA in a gradient from 100:0 to 85:1...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1cccc2ncc3[nH]cnc3c12.c1ccccc1
c1cccc2ncc3nc[nH]c3c12.c1ccccc1
c1cccc2ncc3nc[nH]c3c12.c1ccccc1
HBr.B
null
null
null
CC(C)Cn1cnc2cnc3cccc(Br)c3c21.OB(O)c1ccccc1>>CC(C)Cn1cnc2cnc3cccc(-c4ccccc4)c3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-aa3baeb825a2493d835b1e3bfc26310b
CC(C)Cn1cnc2cnc3cccc(Br)c3c21.CCCOc1ccc(B(O)O)cc1>>CCCOc1ccc(-c2cccc3ncc4ncn(CC(C)C)c4c23)cc1
BrC=1C=2C3=C(C=NC2C=CC1)N=CN3CC(C)C.C(CC)OC1=CC=C(C=C1)B(O)O>>CC(CN1C=NC=2C=NC=3C=CC=C(C3C21)C2=CC=C(C=C2)OCCC)C
Br[c:9]1[cH:10][cH:11][cH:12][c:13]2[n:14][cH:15][c:16]3[n:17][cH:18][n:19]([CH2:20][CH:21]([CH3:22])[CH3:23])[c:24]3[c:25]12.OB(O)[c:8]1[cH:7][cH:6][c:5]([O:4][CH2:3][CH2:2][CH3:1])[cH:27][cH:26]1>>[CH3:1][CH2:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8](-[c:9]2[cH:10][cH:11][cH:12][c:13]3[n:14][cH:15][c:16]4[n:17][cH:18][n:...
CC(C)Cn1cnc2cnc3cccc(Br)c3c21.CCCOc1ccc(B(O)O)cc1
CCCOc1ccc(-c2cccc3ncc4ncn(CC(C)C)c4c23)cc1
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
7641a7375c485375c827a1b7fc577b96303c9dfd51153d2ecc4afa14501f7686
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2cccc3ncc4nc[nH]c4c23)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[c:5]2:[#7;a:6]:[c:7]:[c:8]3:[#7;a:9]:[c:10]:[#7;a:11](-[C:12]):[c:13]:3:[c:14]:2:1.O-B(-O)-[c;H0;D3;+0:15](:[c:16]:[c:17]):[c:18]:[c:19]>>[C:12]-[#7;a:11]1:[c:10]:[#7;a:9]:[c:8]2:[c:7]:[#7;a:6]:[c:5]3:[c:4]:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:15](:[c:16]:[c:17]):[c:18]:[c:19]):...
90
[{"value": 90.0, "product": "CC(CN1C=NC=2C=NC=3C=CC=C(C3C21)C2=CC=C(C=C2)OCCC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
9-Bromo-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinoline (1.0 g, 3.4 mmol) and 4-propoxyphenylboronic acid (1.0 g, 5.5 mmol) were coupled according to Part J of Example 1. The palladium (II) acetate (2.5 mg, 0.011 mmol) was added as a 5 mg/mL solution in toluene. The work-up procedure described in Parts 125–135 was follow...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1cccc2ncc3[nH]cnc3c12.c1ccccc1
c1ccccc1.c1cccc2ncc3[nH]cnc3c12
c1ccccc1.c1cccc2ncc3[nH]cnc3c12
HBr.B
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)C
null
null
CC(C)Cn1cnc2cnc3cccc(Br)c3c21.CCCOc1ccc(B(O)O)cc1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)C>CCCOc1ccc(-c2cccc3ncc4ncn(CC(C)C)c4c23)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5de5ae4e1a584a48b0d2e3a218983a7a
CC#N.CCCOc1ccc(-c2cccc3ncc4ncn(CC(C)C)c4c23)cc1>>CCCOc1ccc(-c2cccc3nc(N)c4ncn(CC(C)C)c4c23)cc1
CC(CN1C=NC=2C=NC=3C=CC=C(C3C21)C2=CC=C(C=C2)OCCC)C.C(C)#N>>CC(CN1C=NC=2C(=NC=3C=CC=C(C3C21)C2=CC=C(C=C2)OCCC)N)C
CC#[N:16].[CH3:1][CH2:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8](-[c:9]2[cH:10][cH:11][cH:12][c:13]3[n:14][cH:15][c:17]4[n:18][cH:19][n:20]([CH2:21][CH:22]([CH3:23])[CH3:24])[c:25]4[c:26]23)[cH:27][cH:28]1>>[CH3:1][CH2:2][CH2:3][O:4][c:5]1[cH:6][cH:7][c:8](-[c:9]2[cH:10][cH:11][cH:12][c:13]3[n:14][c:15]([NH2:16])[c:17]4[n:1...
CC#N.CCCOc1ccc(-c2cccc3ncc4ncn(CC(C)C)c4c23)cc1
CCCOc1ccc(-c2cccc3nc(N)c4ncn(CC(C)C)c4c23)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
668eaaeddba370e0966e8df58804fb8e09839e55608e92b00099a5ce100ab0ef
807c02e8854fa1d85bad1ac2ebd73d5cdddf0728c08cb10c1d1278b952c720d7
c1ccc(-c2cccc3ncc4nc[nH]c4c23)cc1
C-C#[N;H0;D1;+0:1].[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[cH;D2;+0:7]:[#7;a:8]:[c:9]:[c:10]:[c:11]:1:2>>[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6]2:[c:11]:1:[c:10]:[c:9]:[#7;a:8]:[c;H0;D3;+0:7]:2-[NH2;D1;+0:1]
null
[]
null
null
36
HOUR
The method described in Part J of Example 365 was used to oxidize and aminate 1-(2-methylpropyl)-9-(4-propoxyphenyl)-1H-imidazo[4,5-c]quinoline (1.1 g, 3.1 mmol). The amination reaction was stirred for 36 hours. The crude product was purified by HPFC (eluting with chloroform:CMA in a gradient from 100:0 to 70:30) to pr...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
c1cccc2ncc3[nH]cnc3c12
c1nc2ccccc2c2nc[nH]c12
c1ccccc1.c1nc2ccccc2c2nc[nH]c12
Other
null
null
36
CC#N.CCCOc1ccc(-c2cccc3ncc4ncn(CC(C)C)c4c23)cc1>>CCCOc1ccc(-c2cccc3nc(N)c4ncn(CC(C)C)c4c23)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0789ae86abcc4ffcb54afb54fb83337e
CCOC(=O)CC(=O)OCC.Nc1ccccc1Br>>O=C(O)CC(=O)Nc1ccccc1Br
Cl.C(CC(=O)OCC)(=O)OCC.BrC1=C(N)C=CC=C1.C([O-])([O-])=O.[Na+].[Na+]>>BrC1=C(C=CC=C1)NC(CC(=O)O)=O
CCO[C:5]([CH2:4][C:2](=[O:1])[O:3]CC)=[O:6].[NH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][c:13]1[Br:14]>>[O:1]=[C:2]([OH:3])[CH2:4][C:5](=[O:6])[NH:7][c:8]1[cH:9][cH:10][cH:11][cH:12][c:13]1[Br:14]
CCOC(=O)CC(=O)OCC.Nc1ccccc1Br
O=C(O)CC(=O)Nc1ccccc1Br
null
null
CO.O
Protection
OtherReaction
70293d3e8c18e2b6da68ed11b9d6823c24895b8790c14ff32c8b49ced3b12880
29fbc6ece4ea5207c4566380f45c4382f2be045c119b517d772f85d11bb512cc
c1ccccc1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4](=[O;D1;H0:5])-[O;H0;D2;+0:6]-C-C.[NH2;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[O;D1;H0:5]=[C:4](-[OH;D1;+0:6])-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10]
57.3
[{"value": 57.3, "product": "BrC1=C(C=CC=C1)NC(CC(=O)O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
180
CELSIUS
null
null
Diethyl malonate (101 mL, 0.989 mol) and 2-bromoaniline (50.g, 0.291 mol) were combined and heated at 180° C. for six hours. A Dean-Stark trap was used to collect the volatiles. The reaction was allowed to cool to ambient temperature overnight; a precipitate formed. The precipitate was isolated by filtration and combin...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Primary amine
Carboxylic acid.Secondary amide
null
null
c1ccccc1
HO-
CO.O
180
null
CCOC(=O)CC(=O)OCC.Nc1ccccc1Br>CO.O>O=C(O)CC(=O)Nc1ccccc1Br
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-69f9ed9971d84108bc0b47b3fce1fc7f
O=C(O)CC(=O)Nc1ccccc1Br>>Oc1cc(O)c2cccc(Br)c2n1
BrC1=C(C=CC=C1)NC(CC(=O)O)=O.[OH-].[Na+]>>BrC=1C=CC=C2C(=CC(=NC12)O)O
O=[C:4]([CH2:3][C:2](=[O:1])[NH:13][c:12]1[cH:6][cH:7][cH:8][cH:9][c:10]1[Br:11])[OH:5]>>[OH:1][c:2]1[cH:3][c:4]([OH:5])[c:6]2[cH:7][cH:8][cH:9][c:10]([Br:11])[c:12]2[n:13]1
O=C(O)CC(=O)Nc1ccccc1Br
Oc1cc(O)c2cccc(Br)c2n1
null
null
Cl
Aromatic Heterocycle Formation
OtherReaction
9402a7279b29c9d8a731ecc3a1fcf489e5f1179eb567486aae94c816493d85b5
999d168235ae1f4640223947c418a4f3e4605c0e33d865b4a7894f9b30606573
c1ccc2ncccc2c1
O=[C;H0;D3;+0:1](-[O;D1;H1:2])-[CH2;D2;+0:3]-[C;H0;D3;+0:4](=[O;H0;D1;+0:5])-[NH;D2;+0:6]-[c:7](:[c:8]):[cH;D2;+0:9]:[c:10]:[c:11]>>[O;D1;H1:2]-[c;H0;D3;+0:1]1:[cH;D2;+0:3]:[c;H0;D3;+0:4](-[OH;D1;+0:5]):[n;H0;D2;+0:6]:[c:7](:[c:8]):[c;H0;D3;+0:9]:1:[c:10]:[c:11]
91.6
[{"value": 91.6, "product": "BrC=1C=CC=C2C(=CC(=NC12)O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
140
CELSIUS
4
HOUR
N-(2-Bromophenyl)malonamic acid (43 g, 170 mmol), polyphosphoric acid (334 mL of 0.5 M), and hydrochloric acid (444 mL of 1 N) were combined and heated at 140° C. for three hours. The solution was allowed to cool to ambient temperature, and additional hydrochloric acid (603 mL of 1 N) was added. The reaction was stirre...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amide
Aromatic alcohol.Aromatic alcohol
c1ccccc1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HO-
Cl
140
4
O=C(O)CC(=O)Nc1ccccc1Br>Cl>Oc1cc(O)c2cccc(Br)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c8d5b04d3fab4744a5a52f1cf07989d7
O=[N+]([O-])O.Oc1cc(O)c2cccc(Br)c2n1>>O=[N+]([O-])c1c(O)nc2c(Br)cccc2c1O
BrC=1C=CC=C2C(=CC(=NC12)O)O.[N+](=O)(O)[O-].[N+](=O)(O)[O-]>>BrC=1C=CC=C2C(=C(C(=NC12)O)[N+](=O)[O-])O
O[N+:2](=[O:1])[O-:3].[cH:4]1[c:5]([OH:6])[n:7][c:8]2[c:9]([Br:10])[cH:11][cH:12][cH:13][c:14]2[c:15]1[OH:16]>>[O:1]=[N+:2]([O-:3])[c:4]1[c:5]([OH:6])[n:7][c:8]2[c:9]([Br:10])[cH:11][cH:12][cH:13][c:14]2[c:15]1[OH:16]
O=[N+]([O-])O.Oc1cc(O)c2cccc(Br)c2n1
O=[N+]([O-])c1c(O)nc2c(Br)cccc2c1O
null
null
null
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](-[O;D1;H1:10]):[cH;D2;+0:11]:1>>[O;-;D1;H0:2]-[N+;H0;D3:1](=[O;D1;H0:3])-[c;H0;D3;+0:11]1:[c:5](-[O;D1;H1:4]):[c:6]:[c:7]:[#7;a:8]:[c:9]:1-[O;D1;H1:10]
63.9
[{"value": 63.9, "product": "BrC=1C=CC=C2C(=C(C(=NC12)O)[N+](=O)[O-])O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
A modification of the method described in Part D of Example 10 was used to treat 8-bromoquinoline-2,4-diol (10.0 g, 41.6 mmol) with nitric acid (3.6 mL of 11.74 M, 54 mmol). The nitric acid was added at ambient temperature, and then the reaction was heated at 100° C. for one hour, at which time an exotherm occurred. Th...
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HO-
null
100
null
O=[N+]([O-])O.Oc1cc(O)c2cccc(Br)c2n1>>O=[N+]([O-])c1c(O)nc2c(Br)cccc2c1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e4bc21a062524818a009f89c7b32cc59
CC(C)(O)CNc1c(N)c(Cl)nc2c(Br)cccc12.CCOCC(=O)Cl>>CCOCc1nc2cnc3c(Br)cccc3c2n1CC(C)(C)O
NC=1C(=NC2=C(C=CC=C2C1NCC(C)(O)C)Br)Cl.C(C)OCC(=O)Cl.C(C)O.C([O-])([O-])=O.[K+].[K+]>>BrC1=CC=CC=2C3=C(C=NC12)N=C(N3CC(C)(O)C)COCC
Cl[c:8]1[c:7]([NH2:6])[c:17]([NH:18][CH2:19][C:20]([CH3:21])([CH3:22])[OH:23])[c:16]2[c:10]([n:9]1)[c:11]([Br:12])[cH:13][cH:14][cH:15]2.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[c:11]([Br:12])[cH:13][cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][C:20]([CH3:21])([...
CC(C)(O)CNc1c(N)c(Cl)nc2c(Br)cccc12.CCOCC(=O)Cl
CCOCc1nc2cnc3c(Br)cccc3c2n1CC(C)(C)O
null
null
ClCCl.O
Aromatic Heterocycle Formation
OtherReaction
d3d842fa118f2e7920c947aa6ef1a06fae09ab9b42d5d738d2e92f8b7b692f55
bb5ef43dc5e52681475802be44587bc64e5a88f0c1c4eb737da942a7bc33c68c
c1ccc2c(c1)ncc1nc[nH]c12
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[#8:3].Cl-[c;H0;D3;+0:4]1:[#7;a:5]:[c:6]:[c:7]:[c:8](-[NH;D2;+0:9]-[C: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:[cH;D2;+0:4]:[#7;a:5]:[c:6]:[c:7]:[c:8]:2:[n;H0;D3;+0:9]:1-[C:10]-[C:11]
80.8
[{"value": 80.8, "product": "BrC1=CC=CC=2C3=C(C=NC12)N=C(N3CC(C)(O)C)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
40
CELSIUS
36
HOUR
A solution of 1-(3-amino-8-bromo-2-chloroquinolin-4-ylamino)-2-methylpropan-2-ol (4.65 g, 14.4 mmol) and ethoxyacetyl chloride (1.9 mL, 15.8 mmol) in dichloromethane (72 mL) was stirred for one hour at ambient temperature. The solvent was removed under reduced pressure, and ethanol (43 mL), water (29 mL), and potassium...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Aromatic halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1nc2c(cnc3ccccc32)[nH]1
c1nc2c(cnc3ccccc32)[nH]1
HCl
ClCCl.O
40
36
CC(C)(O)CNc1c(N)c(Cl)nc2c(Br)cccc12.CCOCC(=O)Cl>ClCCl.O>CCOCc1nc2cnc3c(Br)cccc3c2n1CC(C)(C)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6ce4ecf087dd4b5e9dfdb947815f2d30
CC1(C)OC[C@@H](CN)O1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>CC1(C)OC[C@@H](CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)O1
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.CC1(OC[C@H](O1)CN)C>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NC[C@H]1OC(OC1)(C)C
[CH3:1][C:2]1([CH3:3])[O:4][CH2:5][C@@H:6]([CH2:7][NH2:8])[O:23]1.Cl[c:9]1[c:10]([N+:11](=[O:12])[O-:13])[cH:14][n:15][c:16]2[cH:17][c:18]([Br:19])[cH:20][cH:21][c:22]12>>[CH3:1][C:2]1([CH3:3])[O:4][CH2:5][C@@H:6]([CH2:7][NH:8][c:9]2[c:10]([N+:11](=[O:12])[O-:13])[cH:14][n:15][c:16]3[cH:17][c:18]([Br:19])[cH:20][cH:21]...
CC1(C)OC[C@@H](CN)O1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
CC1(C)OC[C@@H](CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)O1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2c(NC[C@@H]3COCO3)ccnc2c1
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].[#8:10]-[C:11]-[C:12]-[NH2;D1;+0:13]>>[#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;+0:13]-[C:12]-[C:11]-[#8:10]
88.4
[{"value": 88.4, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NC[C@H]1OC(OC1)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7-Bromo-4-chloro-3-nitroquinoline (22.00 g, 76.52 mmol) was treated with (R)-2,2-dimethyl-1,3-dioxolane-4-methanamine (11.61 g, 114.8 mmol) according to the method described in Part A of Examples 152–156. The crude product was triturated with water (200 mL), isolated by filtration, washed with water, dried, and suspend...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
C1COCO1.c1ccc2ncccc2c1
HCl
null
null
null
CC1(C)OC[C@@H](CN)O1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>CC1(C)OC[C@@H](CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ebe61890eb1d414990c24c6f5dd8ad09
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1C[C@@H]1COC(C)(C)O1.OB(O)c1cccnc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1C[C@@H]1COC(C)(C)O1
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3C[C@H]3OC(OC3)(C)C)COCC.N1=CC(=CC=C1)B(O)O>>CC1(OC[C@H](O1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)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@@H:26]4[CH2:27][O:28][C:29]([CH3:30])([CH3:31])[O:32]4)[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:11]3[cH:12][c:1...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1C[C@@H]1COC(C)(C)O1.OB(O)c1cccnc1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1C[C@@H]1COC(C)(C)O1
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
d23a08b59b246d837a860414fc085402a8d785d2b981e3447d503da913f098ed
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1cncc(-c2ccc3c(c2)ncc2ncn(C[C@@H]4COCO4)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...
65.5
[{"value": 65.5, "product": "CC1(OC[C@H](O1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
(R)-7-Bromo-1-[(2,2-dimethyl-1,3-dioxolan-4-yl)methyl]-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-4-amine (3.0 g, 6.9 mmol) and pyridine-3-boronic acid (1.02 g, 8.27 mmol) were coupled according to the method described in Examples 118–121. The work-up procedure described in Part F of Examples 125–135 was followed. The cr...
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.C1COCO1
HBr.B
null
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1C[C@@H]1COC(C)(C)O1.OB(O)c1cccnc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1C[C@@H]1COC(C)(C)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-81e1d7ec4fba449c82d78b037813b515
CC1(C)OC[C@H](CN)O1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>CC1(C)OC[C@H](CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)O1
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.CC1(OC[C@@H](O1)CN)C.C(C)O>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NC[C@@H]1OC(OC1)(C)C
[CH3:1][C:2]1([CH3:3])[O:4][CH2:5][C@H:6]([CH2:7][NH2:8])[O:23]1.Cl[c:9]1[c:10]([N+:11](=[O:12])[O-:13])[cH:14][n:15][c:16]2[cH:17][c:18]([Br:19])[cH:20][cH:21][c:22]12>>[CH3:1][C:2]1([CH3:3])[O:4][CH2:5][C@H:6]([CH2:7][NH:8][c:9]2[c:10]([N+:11](=[O:12])[O-:13])[cH:14][n:15][c:16]3[cH:17][c:18]([Br:19])[cH:20][cH:21][c...
CC1(C)OC[C@H](CN)O1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
CC1(C)OC[C@H](CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)O1
null
null
ClCCl
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2c(NC[C@H]3COCO3)ccnc2c1
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].[#8:10]-[C:11]-[C:12]-[NH2;D1;+0:13]>>[#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;+0:13]-[C:12]-[C:11]-[#8:10]
96.1
[{"value": 96.1, "product": "BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NC[C@@H]1OC(OC1)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
7-Bromo-4-chloro-3-nitroquinoline (11.00 g, 38.26 mmol) was reacted with (S)-2,2-dimethyl-[1,3]dioxolane-4-methanamine (5.81 g, 57.4 mmol) according to the method described in Part A of Examples 125–135. When the reaction was complete, it was concentrated under reduced pressure, and the residue was stirred with water (...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
C1COCO1.c1ccc2ncccc2c1
HCl
ClCCl
null
null
CC1(C)OC[C@H](CN)O1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>ClCCl>CC1(C)OC[C@H](CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-24769b0edb5146748dcf7bf5bec69837
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1C[C@H]1COC(C)(C)O1.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1C[C@H]1COC(C)(C)O1
BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3C[C@@H]3OC(OC3)(C)C)COCC.B1(OCCCO1)C2=CN=CC=C2>>CC1(OC[C@@H](O1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)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@H:26]4[CH2:27][O:28][C:29]([CH3:30])([CH3:31])[O:32]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:5]1[n:6][c:7]2[c:8]([NH2:9])[n:10][c:11]3[cH:12]...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1C[C@H]1COC(C)(C)O1.c1cncc(B2OCCCO2)c1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1C[C@H]1COC(C)(C)O1
null
null
null
C-C Coupling
Suzuki coupling with boronic esters
2cd1cbe6f17c98cb5223a75d20dfc144a6eae8461c4fe8a7e9cc4bc7ecadb166
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1cncc(-c2ccc3c(c2)ncc2ncn(C[C@H]4COCO4)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...
54.2
[{"value": 54.2, "product": "CC1(OC[C@@H](O1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
(S)-7-Bromo-1-[(2,2-dimethyl-1,3-dioxolan-4-yl)methyl]-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-4-amine (2.65 g, 6.09 mmol) and pyridine-3-boronic acid 1,3-propanediol cyclic ester (1.19 g, 7.30 mmol) were coupled according to the method described in Examples 118–121. The work-up procedure described in Part F of Exampl...
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.C1COCO1
HBr.B
null
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1C[C@H]1COC(C)(C)O1.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1C[C@H]1COC(C)(C)O1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-440aa7395e284f75ac4d4d96d14f7675
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCCCN1C(=O)OC(C)(C)C.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCCCN1C(=O)OC(C)(C)C
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2N(CCCC2)C(=O)OC(C)(C)C)COCC)Br.B1(OCCCO1)C2=CN=CC=C2>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2N(CCCC2)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][CH2:29][CH2:30][N:31]4[C:32](=[O:33])[O:34][C:35]([CH3:36])([CH3:37])[CH3:38])[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]...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCCCN1C(=O)OC(C)(C)C.c1cncc(B2OCCCO2)c1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCCCN1C(=O)OC(C)(C)C
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)ncc2ncn(CC4CCCCN4)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...
70.8
[{"value": 70.8, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2N(CCCC2)C(=O)OC(C)(C)C)COCC)C=2C=NC=CC2", "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)methyl]piperidine-1-carboxylate (4.82 g, 9.30 mmol) and pyridine-3-boronic acid 1,3-propanediol cyclic ester (1.67 g, 10.2 mmol) were coupled according to the method described in Part F of Example 414. Palladium (II) acetate (0.0103 f, 0.046 m...
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
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
null
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCCCN1C(=O)OC(C)(C)C.c1cncc(B2OCCCO2)c1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCCCN1C(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-46965b52963f4a0b906c2734dfbd92bc
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCCCN1.CS(=O)(=O)Cl>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCCCN1S(C)(=O)=O
CS(=O)(=O)Cl.Cl.Cl.Cl.C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC1NCCCC1.C(C)N(CC)CC.CS(=O)(=O)Cl>>C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC1N(CCCC1)S(=O)(=O)C
[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][CH2:29][CH2:30][NH:31]1.Cl[S:32]([CH3:33])(=[O:34])=[O:35]>>[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(-c4cccnc4)ccc3c2n1CC1CCCCN1.CS(=O)(=O)Cl
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCCCN1S(C)(=O)=O
null
null
C(Cl)(Cl)Cl
Acylation
Sulfonamide synthesis (Schotten-Baumann) secondary amine
d63e07b47df62aebedb35134f6d0504cfcbed5ccfdec31c2c42bba6875c15fe7
b7aca5a5d690b0846685a854bc946849e1041bfc3965161290b5ffb2821af09e
c1cncc(-c2ccc3c(c2)ncc2ncn(CC4CCCCN4)c23)c1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6](-[C:7])-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:5]-[C:6](-[C:7])-[N;H0;D3;+0:8](-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4])-[C:9]-[C:10]
34.9
[{"value": 34.9, "product": "C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)C=2C=NC=CC2)N)N1)CC1N(CCCC1)S(=O)(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of 2-ethoxymethyl-1-(piperidin-2-ylmethyl)-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine trihydrochloride (0.60 g, 1.1 mmol) and triethylamine (0.79 mL, 5.7 mmol) in chloroform (50 mL) was cooled to 4° C. Methanesulfonyl chloride (0.12 mL, 1.5 mmol) was added, and the reaction was allowed to warm to amb...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Sulfonyl halide
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.C1CC[NH]CC1
HCl
C(Cl)(Cl)Cl
null
8
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCCCN1.CS(=O)(=O)Cl>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CC1CCCCN1S(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e290789573584e50a29ba8fd5e830722
CC(C)(C)OC(=O)NCc1ccc(CN)cc1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>CC(C)(C)OC(=O)NCc1ccc(CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)cc1
C(=O)(OC(C)(C)C)NCC1=CC=C(C=C1)CN.BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.C(C)N(CC)CC>>C(C)(C)(C)OC(NCC1=CC=C(C=C1)CNC1=C(C=NC2=CC(=CC=C12)Br)[N+](=O)[O-])=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([CH2:14][NH2:15])[cH:30][cH:31]1.Cl[c:16]1[c:17]([N+:18](=[O:19])[O-:20])[cH:21][n:22][c:23]2[cH:24][c:25]([Br:26])[cH:27][cH:28][c:29]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([CH...
CC(C)(C)OC(=O)NCc1ccc(CN)cc1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
CC(C)(C)OC(=O)NCc1ccc(CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)cc1
null
null
ClCCl
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
45e8470a78418ade39424f40732aa5ecf6717a7e5d47830a67429c5970ebd551
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(CNc2ccnc3ccccc23)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].[NH2;D1;+0:10]-[C:11]-[c: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;+0:10]-[C:11]-[c:12]
93.4
[{"value": 93.4, "product": "C(C)(C)(C)OC(NCC1=CC=C(C=C1)CNC1=C(C=NC2=CC(=CC=C12)Br)[N+](=O)[O-])=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
1-(N-BOC-aminomethyl)-4-(aminomethyl)benzene (5.0 g, 21 mmol) in dichloromethane (50 mL) was added dropwise to a mixture of 7-bromo-4-chloro-3-nitroquinoline (5.81 g, 20 mmol) and triethylamine (5.63 mL) in dichloromethane (60 mL). The reaction was stirred for 16 hours and then washed sequentially with water and satura...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccccc1.c1ccc2ncccc2c1
HCl
ClCCl
null
16
CC(C)(C)OC(=O)NCc1ccc(CN)cc1.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>ClCCl>CC(C)(C)OC(=O)NCc1ccc(CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e14b4f690e7d423e92497dc07775b581
CC(C)(C)OC(=O)NCc1ccc(CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)cc1>>CC(C)(C)OC(=O)NCc1ccc(CNc2c(N)cnc3cc(Br)ccc23)cc1
C([O-])([O-])=O.[K+].[K+].S(=O)([O-])S(=O)[O-].[Na+].[Na+].C(C)(C)(C)OC(NCC1=CC=C(C=C1)CNC1=C(C=NC2=CC(=CC=C12)Br)[N+](=O)[O-])=O>>C(C)(C)(C)OC(NCC1=CC=C(C=C1)CNC1=C(C=NC2=CC(=CC=C12)Br)N)=O
O=[N+:18]([O-])[c:17]1[c:16]([NH:15][CH2:14][c:13]2[cH:12][cH:11][c:10]([CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[cH:29][cH:28]2)[c:27]2[c:21]([n:20][cH:19]1)[cH:22][c:23]([Br:24])[cH:25][cH:26]2>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([CH2:14][NH:1...
CC(C)(C)OC(=O)NCc1ccc(CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)cc1
CC(C)(C)OC(=O)NCc1ccc(CNc2c(N)cnc3cc(Br)ccc23)cc1
null
CC[N+]1=CC=C(C=C1)C2=CC=[N+](C=C2)CC.[Br-].[Br-]
ClCCl.O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(CNc2ccnc3ccccc23)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]
100.5
[{"value": 100.5, "product": "C(C)(C)(C)OC(NCC1=CC=C(C=C1)CNC1=C(C=NC2=CC(=CC=C12)Br)N)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
Ethyl viologen dibromide (0.069 g, 0.18 mmol), potassium carbonate (12.76 g, 92 mmol) in water (55mL), and sodium hydrosulfite (11.25 g, 65 mmol) in water (55mL) were added sequentially to a solution of tert-butyl{4-[(7-bromo-3-nitroquinolin-4-ylamino)methyl]benzyl}carbamate (9.0 g, 18.5 mmol) in dichloromethane (110 m...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccc2ncccc2c1
Other
CC[N+]1=CC=C(C=C1)C2=CC=[N+](C=C2)CC.[Br-].[Br-].ClCCl.O
null
20
CC(C)(C)OC(=O)NCc1ccc(CNc2c([N+](=O)[O-])cnc3cc(Br)ccc23)cc1>CC[N+]1=CC=C(C=C1)C2=CC=[N+](C=C2)CC.[Br-].[Br-].ClCCl.O>CC(C)(C)OC(=O)NCc1ccc(CNc2c(N)cnc3cc(Br)ccc23)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8944d4bc581b4c2091b717fc29f8e6a3
CC(C)(C)OC(=O)NCc1ccc(CNc2c(N)cnc3cc(Br)ccc23)cc1.CCOCC(=O)Cl>>CCOCc1nc2cnc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
NC=1C=NC2=CC(=CC=C2C1NCC1=CC=C(CNC(OC(C)(C)C)=O)C=C1)Br.C(C)N(CC)CC.C(C)OCC(=O)Cl>>C(C)(C)(C)OC(NCC1=CC=C(C=C1)CN1C(=NC=2C=NC=3C=C(C=CC3C21)Br)COCC)=O
[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]1[cH:21][cH:22][c:23]([CH2:24][NH:25][C:26](=[O:27])[O:28][C:29]([CH3:30])([CH3:31])[CH3:32])[cH:33][cH:34]1.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...
CC(C)(C)OC(=O)NCc1ccc(CNc2c(N)cnc3cc(Br)ccc23)cc1.CCOCC(=O)Cl
CCOCc1nc2cnc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
null
null
ClCCl
Aromatic Heterocycle Formation
OtherReaction
101a087a520f159c722ba3d78ed38f5c3c1cf154206e5edbeb1e6397c929560f
56ef83dfadec35a1cf1db968b807e178cc4924ce15bf36d774883783cef0f450
c1ccc(Cn2cnc3cnc4ccccc4c32)cc1
Cl-[C;H0;D3;+0:1](=O)-[C:2]-[#8:3].[NH2;D1;+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]
35
[{"value": 35.0, "product": "C(C)(C)(C)OC(NCC1=CC=C(C=C1)CN1C(=NC=2C=NC=3C=C(C=CC3C21)Br)COCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
tert-Butyl {4-[(3-amino-7-bromoquinolin-4-ylamino)methyl]benzyl}carbamate (8.46 g, 18.5 mmol), triethylamine (2.25 mL) and dichloromethane (92 mL) were combined. Ethoxyacetyl chloride (2.92 g, 24 mmol) was added dropwise to the mixture. The reaction was stirred for an additional 1.5 hours and then concentrated under re...
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
HCl
ClCCl
null
1.5
CC(C)(C)OC(=O)NCc1ccc(CNc2c(N)cnc3cc(Br)ccc23)cc1.CCOCC(=O)Cl>ClCCl>CCOCc1nc2cnc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-aa8698d39a6b418ab64bf6c776047c64
CCOCc1nc2cnc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1.[NH4+]>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
C1(=CC=C(C=C1)S(=O)(=O)Cl)C.ClC=1C=C(C(=O)OO)C=CC1.C(C)(C)(C)OC(NCC1=CC=C(C=C1)CN1C(=NC=2C=NC=3C=C(C=CC3C21)Br)COCC)=O.[OH-].[NH4+]>>C(C)(C)(C)OC(NCC1=CC=C(C=C1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)=O
[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][c:21]1[cH:22][cH:23][c:24]([CH2:25][NH:26][C:27](=[O:28])[O:29][C:30]([CH3:31])([CH3:32])[CH3:33])[cH:34][cH:35]1.[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...
CCOCc1nc2cnc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1.[NH4+]
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
null
null
C(Cl)(Cl)Cl
Functional Group Addition
OtherReaction
dc63235befaaf41df35292b6862b726098d8e1b79a2cef881f35b7cf9ff16606
d69ce1fde4173969963123914389bef807fad83b73b8a587195a7122d5cdf1d2
c1ccc(Cn2cnc3cnc4ccccc4c32)cc1
[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
1
HOUR
3-Chloroperoxybenzoic acid (2.91 g, 9.3 mmol, 55% pure) was added to a solution of tert-butyl[4-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-ylmethyl)benzyl]carbamate (3.2 g, 6.1 mmol) in chloroform (60 mL). The reaction was stirred for 1 hour and then cooled with an ice bath. Ammonium hydroxide (40 mL) was adde...
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.c1ccccc1
null
C(Cl)(Cl)Cl
null
1
CCOCc1nc2cnc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1.[NH4+]>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-730080668d58495bb46b128bad4a9aa6
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1.c1cncc(B2OCCCO2)c1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
C(C)(C)(C)OC(NCC1=CC=C(C=C1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)=O.B1(OCCCO1)C2=CN=CC=C2.C([O-])([O-])=O.[Na+].[Na+].C(CC)O>>C(C)(C)(C)OC(NCC1=CC=C(C=C1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)=O
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]4[cH:27][cH:28][c:29]([CH2:30][NH:31][C:32](=[O:33])[O:34][C:35]([CH3:36])([CH3:37])[CH3:38])[cH:39][cH:40]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]...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1.c1cncc(B2OCCCO2)c1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
null
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1
O
C-C Coupling
Suzuki coupling with boronic esters
2cd1cbe6f17c98cb5223a75d20dfc144a6eae8461c4fe8a7e9cc4bc7ecadb166
48892094855745f5c51f8910c27ce7c101e08ad3f9da2a58d5512e3d9c1b432f
c1ccc(Cn2cnc3cnc4cc(-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.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...
64.1
[{"value": 64.1, "product": "C(C)(C)(C)OC(NCC1=CC=C(C=C1)CN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
105
CELSIUS
null
null
tert-Butyl[4-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-ylmethyl)benzyl]carbamate (1.15 g, 2.1 mmol), triphenylphosphine (0.005 g), pyridine-3-boronic acid 1,3-propanediol cyclic ester (0.365 g, 2.2 mmol), and n-propanol (3.67 mL) were combined. Aqueous sodium carbonate (2M, 1.12 mL) and water (0.6 mL)...
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.c1ccccc1
HBr.B
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.O
105
null
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1.c1cncc(B2OCCCO2)c1>C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.O>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4c2681be703e4a42a213e914545c842e
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CN)cc1
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2=CC=C(CNC(OC(C)(C)C)=O)C=C2)COCC)C=2C=NC=CC2>>NCC1=CC=C(CN2C(=NC=3C(=NC=4C=C(C=CC4C32)C=3C=NC=CC3)N)COCC)C=C1
CC(C)(C)OC(=O)[NH:31][CH2:30][c:29]1[cH:28][cH:27][c: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)[cH:33][cH:32]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[c...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CN)cc1
null
null
Cl
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc(Cn2cnc3cnc4cc(-c5cccnc5)ccc4c32)cc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[c:3]>>[NH2;D1;+0:1]-[C:2]-[c:3]
97.9
[{"value": 97.9, "product": "NCC1=CC=C(CN2C(=NC=3C(=NC=4C=C(C=CC4C32)C=3C=NC=CC3)N)COCC)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
tert-Butyl {4-[4-amino-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-1-ylmethyl]benzyl}carbamate (0.660 g) was added to ethanolic hydrogen chloride (4M, 10 mL) and the solution was heated at reflux temperature for 30 minutes. The reaction was cooled to room temperature and concentrated under reduced pressur...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.c1ccccc1
HO-
Cl
null
null
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNC(=O)OC(C)(C)C)cc1>Cl>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CN)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-eb0c87782d154fc1a5d50dcca884829e
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CN)cc1.CS(=O)(=O)Cl>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNS(C)(=O)=O)cc1
CS(=O)(=O)Cl.NCC1=CC=C(CN2C(=NC=3C(=NC=4C=C(C=CC4C32)C=3C=NC=CC3)N)COCC)C=C1.C([O-])([O-])=O.[Na+].[Na+]>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2=CC=C(CNS(=O)(=O)C)C=C2)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][c:26]1[cH:27][cH:28][c:29]([CH2:30][NH2:31])[cH:36][cH:37]1.Cl[S:32]([CH3:33])(=[O:34])=[O:35]>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[n:6][c:7]2[c:8]([NH...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CN)cc1.CS(=O)(=O)Cl
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNS(C)(=O)=O)cc1
null
null
ClCCl
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
c1ccc(Cn2cnc3cnc4cc(-c5cccnc5)ccc4c32)cc1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[NH2;D1;+0:5]-[C:6]-[c:7]>>[C;D1;H3:2]-[S;H0;D4;+0:1](=[O;D1;H0:3])(=[O;D1;H0:4])-[NH;D2;+0:5]-[C:6]-[c:7]
38.7
[{"value": 38.7, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC2=CC=C(CNS(=O)(=O)C)C=C2)COCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
Methanesulfonyl chloride (0.13 mL, 1.7 mmol) was added dropwise to a mixture of 1-(4-aminomethylbenzyl)-2-ethoxymethyl-7-(pyridin-3-yl)-1H-imidazo[4,5-c]quinolin-4-amine (0.520 g, 1.2 mmol) in dichloromethane (10 mL). The reaction was stirred for 16 hours and then saturated aqueous sodium carbonate was added. The layer...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.c1ccccc1
HCl
ClCCl
null
16
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CN)cc1.CS(=O)(=O)Cl>ClCCl>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1Cc1ccc(CNS(C)(=O)=O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e6aae422c5174d3cb16088d3a37e9cb7
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN.CN(C)CCOC(c1ccccc1)c1ccc(C(=O)O)cc1>>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)c1ccc(C(OCCN(C)C)c2ccccc2)cc1
CN(CCOC(C1=CC=C(C(=O)O)C=C1)C1=CC=CC=C1)C.ON1N=NC2=C1C=CC=C2.NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)C=2C=NC=CC2)N)COCC.Cl.CN(CCCN=C=NCC)C>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(C2=CC=C(C=C2)C(C2=CC=CC=C2)OCCN(C)C)=O)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][CH2:27][CH2:28][NH2:29].O[C:30](=[O:31])[c:32]1[cH:33][cH:34][c:35]([CH:36]([O:37][CH2:38][CH2:39][N:40]([CH3:41])[CH3:42])[c:43]2[cH:44][cH...
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN.CN(C)CCOC(c1ccccc1)c1ccc(C(=O)O)cc1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)c1ccc(C(OCCN(C)C)c2ccccc2)cc1
null
null
CC(=O)N(C)C.C(Cl)(Cl)Cl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(NCCCCn1cnc2cnc3cc(-c4cccnc4)ccc3c21)c1ccc(Cc2ccccc2)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
61.9
[{"value": 61.9, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(C2=CC=C(C=C2)C(C2=CC=CC=C2)OCCN(C)C)=O)COCC)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
A mixture of 4-[(2-dimethylaminoethoxy)phenylmethyl]benzoic acid (0.433 g) and 1-hydroxybenzotriazole (0.196 g) in chloroform (7 mL) was cooled to 0° C. and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.277 g) was added in small portions over a 2 minute period. The mixture was stirred for 1 hour and th...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1.c1ccccc1.c1ccccc1
HO-
CC(=O)N(C)C.C(Cl)(Cl)Cl
0
1
CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCN.CN(C)CCOC(c1ccccc1)c1ccc(C(=O)O)cc1>CC(=O)N(C)C.C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(-c4cccnc4)ccc3c2n1CCCCNC(=O)c1ccc(C(OCCN(C)C)c2ccccc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a763b5a33d5f4a50b6f144f670dad872
NCCN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>>NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])Cl.C(CN)N>>BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCN
[NH2:1][CH2:2][CH2:3][NH2:4].Cl[c:5]1[c:6]([N+:7](=[O:8])[O-:9])[cH:10][n:11][c:12]2[cH:13][c:14]([Br:15])[cH:16][cH:17][c:18]12>>[NH2:1][CH2:2][CH2:3][NH:4][c:5]1[c:6]([N+:7](=[O:8])[O-:9])[cH:10][n:11][c:12]2[cH:13][c:14]([Br:15])[cH:16][cH:17][c:18]12
NCCN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl
NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
null
null
CN(C)C=O
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]
null
[]
null
null
8
HOUR
A solution of 7-bromo-4-chloro-3-nitroquinoline (143.8 g, 0.5 mol) in 800 mL warm DMF was added to a stirred solution of ethylenediamine in 200 mL DMF at room temperature; the reaction was stirred at room temperature overnight. The reaction was quenched with 2 L water and stirred for an additional hour. Additional wate...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2ncccc2c1
c1ccc2ncccc2c1
c1ccc2ncccc2c1
HCl
CN(C)C=O
null
8
NCCN.O=[N+]([O-])c1cnc2cc(Br)ccc2c1Cl>CN(C)C=O>NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b33109869e254d76aed04997a8636ff6
CS(=O)(=O)NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>>CS(=O)(=O)NCCNc1c(N)cnc2cc(Br)ccc12
BrC1=CC=C2C(=C(C=NC2=C1)[N+](=O)[O-])NCCNS(=O)(=O)C>>NC=1C=NC2=CC(=CC=C2C1NCCNS(=O)(=O)C)Br
O=[N+:11]([O-])[c:10]1[c:9]([NH:8][CH2:7][CH2:6][NH:5][S:2]([CH3:1])(=[O:3])=[O:4])[c:20]2[c:14]([n:13][cH:12]1)[cH:15][c:16]([Br:17])[cH:18][cH:19]2>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][CH2:6][CH2:7][NH:8][c:9]1[c:10]([NH2:11])[cH:12][n:13][c:14]2[cH:15][c:16]([Br:17])[cH:18][cH:19][c:20]12
CS(=O)(=O)NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12
CS(=O)(=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]
null
[]
null
null
8
HOUR
An 8 L stainless steel Parr vessel was charged with N-[2-(7-bromo-3-nitroquinolin-4-ylamino)ethyl]methanesulfonamide (61 g), 5% Pt/C catalyst (6.0 g) and acetonitrile (3 L). The vessel was evacuated, filled with hydrogen (45 psi, 3.1×105 Pa), and shaken at ambient temperature overnight. The reaction mixture was filtere...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2ncccc2c1
Other
[Pt].C(C)#N
null
8
CS(=O)(=O)NCCNc1c([N+](=O)[O-])cnc2cc(Br)ccc12>[Pt].C(C)#N>CS(=O)(=O)NCCNc1c(N)cnc2cc(Br)ccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ab7b1d1d5bf34e299a5c6ee23d6d3cfb
CCCCC(=O)Cl.CS(=O)(=O)NCCNc1c(N)cnc2cc(Br)ccc12>>CCCCc1nc2cnc3cc(Br)ccc3c2n1CCNS(C)(=O)=O
NC=1C=NC2=CC(=CC=C2C1NCCNS(=O)(=O)C)Br.C(CCCC)(=O)Cl>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCNS(=O)(=O)C)CCCC
O=[C:5](Cl)[CH2:4][CH2:3][CH2:2][CH3:1].[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][CH2:20][NH:21][S:22]([CH3:23])(=[O:24])=[O:25]>>[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][CH2:20...
CCCCC(=O)Cl.CS(=O)(=O)NCCNc1c(N)cnc2cc(Br)ccc12
CCCCc1nc2cnc3cc(Br)ccc3c2n1CCNS(C)(=O)=O
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]-[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
1.5
HOUR
To a stirred solution of N-[2-(3-amino-7-bromoquinolin-4-ylamino)ethyl]methanesulfonamide (46.4 g, 0.129 mol) in 1000 mL pyridine was slowly added valeryl chloride (1.1 equivalents). After 1.5 hours the mixture was yellow and turbid. The reaction mixture was then heated at reflux for 12 hours, allowed to cool to ambien...
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
1.5
CCCCC(=O)Cl.CS(=O)(=O)NCCNc1c(N)cnc2cc(Br)ccc12>N1=CC=CC=C1>CCCCc1nc2cnc3cc(Br)ccc3c2n1CCNS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-633c6df4f26b4aa19b24d536d897844f
CCCCc1nc2cnc3cc(Br)ccc3c2n1CCNS(C)(=O)=O.[NH4+]>>CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNS(C)(=O)=O
C1(=CC=C(C=C1)S(=O)(=O)Cl)C.ClC=1C=C(C(=O)OO)C=CC1.BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCNS(=O)(=O)C)CCCC.C([O-])([O-])=O.[K+].[K+].[OH-].[NH4+]>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNS(=O)(=O)C)CCCC)Br
[CH3:1][CH2:2][CH2:3][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][NH:22][S:23]([CH3:24])(=[O:25])=[O:26].[NH4+:9]>>[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]([Br:14])[cH:15][cH:16][c:17]3[c:18]2[n:19]1[CH2...
CCCCc1nc2cnc3cc(Br)ccc3c2n1CCNS(C)(=O)=O.[NH4+]
CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNS(C)(=O)=O
null
null
ClCCl.O
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 (1.0 equivalent of 50% pure material) was added to a solution of N-[2-(7-bromo-2-butyl-1H-imidazo[4,5-c]quinolin-1-yl)ethyl]methanesulfonamide (44 g, 103.4 mmol) in 1000 mL dichloromethane. After 2 hours, concentrated ammonium hydroxide solution (600 mL) was added. The reaction was stirred fo...
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.O
null
2
CCCCc1nc2cnc3cc(Br)ccc3c2n1CCNS(C)(=O)=O.[NH4+]>ClCCl.O>CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3930a4c368c440b2ab323231484fcfea
C=C[B-](F)(F)F.CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNS(C)(=O)=O>>C=Cc1ccc2c(c1)nc(N)c1nc(CCCC)n(CCNS(C)(=O)=O)c12
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNS(=O)(=O)C)CCCC)Br.C(=C)[B-](F)(F)F.[K+]>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCNS(=O)(=O)C)CCCC)C=C
F[B-](F)(F)[CH:2]=[CH2:1].Br[c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[n:9][c:10]([NH2:11])[c:12]1[n:13][c:14]([CH2:15][CH2:16][CH2:17][CH3:18])[n:19]([CH2:20][CH2:21][NH:22][S:23]([CH3:24])(=[O:25])=[O:26])[c:27]21>>[CH2:1]=[CH:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[n:9][c:10]([NH2:11])[c:12]1[n:13][c:14]([CH2:15][CH2:1...
C=C[B-](F)(F)F.CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNS(C)(=O)=O
C=Cc1ccc2c(c1)nc(N)c1nc(CCCC)n(CCNS(C)(=O)=O)c12
null
null
null
Functional Group Interconversion
OtherReaction
b6174e4193e02027d22a36dfa7ee1eca16a8f84c44e86ec780137145ed7eacc0
493c526dad91fdaab0a79ca6b28939f7e66256ca7a9e4efc8dfd07eebbd72256
c1ccc2c(c1)ncc1nc[nH]c12
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]2:[c:5](:[#7;a:6]):[c:7](:[#7;a:8]):[c:9]:[#7;a:10]:[c:11]:2:[c:12]:1.F-[B-](-F)(-F)-[CH;D2;+0:13]=[C;D1;H2:14]>>[#7;a:8]:[c:7]1:[c:9]:[#7;a:10]:[c:11]2:[c:12]:[c;H0;D3;+0:1](-[CH;D2;+0:13]=[C;D1;H2:14]):[c:2]:[c:3]:[c:4]:2:[c:5]:1:[#7;a:6]
null
[]
null
null
null
null
N-[2-(4-Amino-7-bromo-2-butyl-1H-imidazo[4,5-c]quinolin-1-yl)ethyl]methanesulfonamide was coupled with potassium vinyltrifluoroborate according to the procedure described in Part D of Examples 440–455 and recrystallized from acetonitrile to provide N-[2-(4-amino-2-butyl-7-vinyl-1H-imidazo[4,5-c]quinolin-1-yl)ethyl]meth...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Vinyl
Vinyl
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
Br-.B
null
null
null
C=C[B-](F)(F)F.CCCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCNS(C)(=O)=O>>C=Cc1ccc2c(c1)nc(N)c1nc(CCCC)n(CCNS(C)(=O)=O)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9312b9100a3448fd880c4a1e4f95c690
CCCNC(=O)NCCNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl>>CCCNC(=O)NCCn1c(COCC)nc2cnc3cc(Br)ccc3c21
NC=1C=NC2=CC(=CC=C2C1NCCNC(=O)NCCC)Br.C(C)OCC(=O)Cl>>BrC=1C=CC=2C3=C(C=NC2C1)N=C(N3CCNC(=O)NCCC)COCC
[CH3:1][CH2:2][CH2:3][NH:4][C:5](=[O:6])[NH:7][CH2:8][CH2:9][NH:10][c:27]1[c:17]([NH2:16])[cH:18][n:19][c:20]2[cH:21][c:22]([Br:23])[cH:24][cH:25][c:26]21.O=[C:11](Cl)[CH2:12][O:13][CH2:14][CH3:15]>>[CH3:1][CH2:2][CH2:3][NH:4][C:5](=[O:6])[NH:7][CH2:8][CH2:9][n:10]1[c:11]([CH2:12][O:13][CH2:14][CH3:15])[n:16][c:17]2[cH...
CCCNC(=O)NCCNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl
CCCNC(=O)NCCn1c(COCC)nc2cnc3cc(Br)ccc3c21
null
null
N1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
092888ef5709db41360ea7e61766d8be84b90a21a3bf7772e6af19a215999134
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]
null
[]
80
CELSIUS
1.5
HOUR
To a stirred solution of 1-[2-(3-amino-7-bromoquinolin-4-ylamino)ethyl]-3-(2-methylethyl)urea (27.2 g, 0.0743 mol) in 600 mL pyridine was slowly added ethoxyacetyl chloride (1.1 equivalents). After 1.5 hours the mixture was yellow and turbid. The reaction mixture was then heated at 80° C. for 12 hours and then concentr...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine.Secondary amine
null
c1ccc2ncccc2c1
c1ccc2c(c1)ncc1nc[nH]c12
c1ccc2c(c1)ncc1nc[nH]c12
HCl
N1=CC=CC=C1
80
1.5
CCCNC(=O)NCCNc1c(N)cnc2cc(Br)ccc12.CCOCC(=O)Cl>N1=CC=CC=C1>CCCNC(=O)NCCn1c(COCC)nc2cnc3cc(Br)ccc3c21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-02f3772b166949dc9620d2ef20591eba
C=Cc1ccccn1.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCOC>>CCOCc1nc2c(N)nc3cc(/C=C/c4ccccn4)ccc3c2n1CCCOC
C1(=C(C=CC=C1)P(C1=C(C=CC=C1)C)C1=C(C=CC=C1)C)C.C(C)N(CC)CC.C(=C)C1=NC=CC=C1.BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CCCOC)COCC>>C(C)OCC=1N(C2=C(C(=NC=3C=C(C=CC23)\C=C\C2=NC=CC=C2)N)N1)CCCOC
[CH2:14]=[CH:15][c:16]1[cH:17][cH:18][cH:19][cH:20][n: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][O:3][CH2:2][CH3:1])[n:26]([CH2:27][CH2:28][CH2:29][O:30][CH3:31])[c:25]3[c:24]2[cH:23][cH:22]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](/[CH:14]=[CH:...
C=Cc1ccccn1.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCOC
CCOCc1nc2c(N)nc3cc(/C=C/c4ccccn4)ccc3c2n1CCCOC
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
C1(=CC=CC=C1)C
C-C Coupling
Heck terminal vinyl
17b6ed2dfc150cdb58934d18ea4782cc332e8e1eab0cb0866f204b219967b10e
4b186811a4930853b446d93d9faa39b267bddb9ce0b8021bda5c5a3b2bc69f0b
C(=C/c1ccccn1)\c1ccc2c(c1)ncc1nc[nH]c12
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.[#7;a:13]:[c:14]-[C:15]=[CH2;D1;+0:16]>>[#7;a:13]:[c:14]/[C:15]=[CH;D2;+0:16]/[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
null
[]
120
CELSIUS
null
null
A thick walled glass tube, equipped with magnetic stir-bar, was charged with toluene (20 mL/g), palladium (II) acetate (0.1 equivalents), tri-ortho-tolylphosphine (0.3 equivalents), triethylamine (3.0 equivalents), 2-vinylpyridine (1.0 equivalent), and 7-bromo-2-ethoxymethyl-1-(3-methoxypropyl)-1H-imidazo[4,5-c]quinoli...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Vinyl
null
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccncc1
HBr
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)C
120
null
C=Cc1ccccn1.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCOC>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)C>CCOCc1nc2c(N)nc3cc(/C=C/c4ccccn4)ccc3c2n1CCCOC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-80cf92620b04461a88045e5db197cc1b
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C>>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN
Cl.NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(OC(C)(C)C)=O)CCC)Br.[OH-].[Na+]>>NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)CCC
CC(C)(C)OC(=O)[NH:23][CH2:22][CH2:21][CH2:20][CH2:19][n:18]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]([Br:13])[cH:14][cH:15][c:16]3[c:17]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]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][CH2:...
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C
CCCc1nc2c(N)nc3cc(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]
null
[]
null
null
30
MINUTE
Concentrated hydrochloric acid (˜15 mL) was added to a suspension of tert-butyl [4-(4-amino-7-bromo-2-propyl-1H-imidazo[4,5-c]quinolin-1-yl)butyl]carbamate (3.19 g, 6.7 mmol) in ethanol (6.4 mL), and the reaction was stirred for 30 minutes. The reaction was adjusted to pH 13 with the addition of 50% aqueous sodium hydr...
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
0.5
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C>C(C)O>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e76e69c5bfb14c809cb53c5b0ed0f7aa
CC(C)N=C=O.CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN>>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)NC(C)C
C(C)(C)N=C=O.C(C)(C)N=C=O.NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)CCC.C(C)(C)N=C=O>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(=O)NC(C)C)CCC)Br
[C:24](=[O:25])=[N:26][CH:27]([CH3:28])[CH3:29].[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]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][CH2:21][CH2:22][NH2:23]>>[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]([Br:13])[cH:14][cH:15][c:16]3[c...
CC(C)N=C=O.CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)NC(C)C
null
null
C(Cl)(Cl)Cl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
c1ccc2c(c1)ncc1nc[nH]c12
[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]
81.4
[{"value": 81.4, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(=O)NC(C)C)CCC)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
A suspension of 1-(4-aminobutyl)-7-bromo-2-propyl-1H-imidazo[4,5-c]quinolin-4-amine (2.00 g, 5.3 mmol) in chloroform (20 mL) was cooled to 0° C., and a solution of isopropyl isocyanate (5.3 mmol) in chloroform (3 mL/g) was added slowly over a period of eight minutes. After one hour, additional isopropyl isocyanate (0.5...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccc2c(c1)ncc1[nH]cnc12
null
C(Cl)(Cl)Cl
0
1
CC(C)N=C=O.CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN>C(Cl)(Cl)Cl>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)NC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8ff2852322ff44bfbfb34c188b4e6d7d
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.O=C(Cl)C1CCCC1>>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)C1CCCC1
NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)CCC.C(C)N(CC)CC.C1(CCCC1)C(=O)Cl>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(=O)C2CCCC2)CCC)Br
[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]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][CH2:21][CH2:22][NH2:23].Cl[C:24](=[O:25])[CH:26]1[CH2:27][CH2:28][CH2:29][CH2:30]1>>[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]([Br:13])[cH:14][cH:1...
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.O=C(Cl)C1CCCC1
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)C1CCCC1
null
null
C(Cl)(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
O=C(NCCCCn1cnc2cnc3ccccc3c21)C1CCCC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5]
49.9
[{"value": 49.9, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(=O)C2CCCC2)CCC)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
A suspension of 1-(4-aminobutyl)-7-bromo-2-propyl-1H-imidazo[4,5-c]quinolin-4-amine (2.42 g, 6.4 mmol) and triethylamine (0.99 mL, 7.1 mmol) in chloroform (240 mL) was cooled to 0° C., and cyclopentanecarbonyl chloride (0.78 mL, 6.4 mmol) was added dropwise over a period of five minutes. The reaction was stirred for te...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2c(c1)ncc1[nH]cnc12.C1CCCC1
HCl
C(Cl)(Cl)Cl
0
null
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.O=C(Cl)C1CCCC1>C(Cl)(Cl)Cl>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)C1CCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5d181d92d4be45a0a6fa4f4664e4e646
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCNCC1.O=C(Cl)N1CCOCC1>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)N2CCOCC2)CC1
Cl.Cl.BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC3CCNCC3)COCC.C(C)N(CC)CC.N1(CCOCC1)C(=O)Cl>>BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC3CCN(CC3)C(=O)N3CCOCC3)COCC
[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:17]3[c:18]2[n:19]1[CH2:20][CH:21]1[CH2:22][CH2:23][NH:24][CH2:33][CH2:34]1.Cl[C:25](=[O:26])[N:27]1[CH2:28][CH2:29][O:30][CH2:31][CH2:32]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[...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCNCC1.O=C(Cl)N1CCOCC1
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)N2CCOCC2)CC1
null
null
C(Cl)(Cl)Cl
Acylation
N-alkylation of secondary amines with alkyl halides
2f6d0cf68900b13baad66104d6931c4ea135cb252da038c5d876a65827ece4fa
353c6e1db25433862a8bcf26ca332f6abeb45cb685806584bc65f8cfcb712540
O=C(N1CCOCC1)N1CCC(Cn2cnc3cnc4ccccc4c32)CC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C:4])-[C:5].[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C:4])-[C:5])-[C:9]-[C:10]
84.6
[{"value": 84.6, "product": "BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC3CCN(CC3)C(=O)N3CCOCC3)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of 7-bromo-2-ethoxymethyl-1-(piperidin-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-4-amine dihydrochloride (4.0 g, 8.1 mmol) and triethylamine (5.67 mL, 40.7 mmol) in chloroform (300 mL) was cooled to 0° C., and 4-morpholinecarbonyl chloride (0.95 mL, 8.1 mmol) was added dropwise. The reaction was allowed to warm ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Tertiary amide.Secondary amine
Urea
C1CCNCC1
C1CC[NH]CC1
c1ccc2c(c1)ncc1[nH]cnc12.C1CC[NH]CC1.C1COCC[NH]1
HCl
C(Cl)(Cl)Cl
null
8
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCNCC1.O=C(Cl)N1CCOCC1>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)N2CCOCC2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-15a5760ecf63496191c81786fd202801
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN
[OH-].[Na+].C([O-])(O)=O.[Na+].Cl.C(C)(C)(C)OC(NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC)=O>>NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC
CC(C)(C)OC(=O)[NH:24][CH2:23][CH2:22][CH2:21][CH2:20][n:19]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]([Br:14])[cH:15][cH:16][c:17]3[c:18]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]([Br:14])[cH:15][cH:16][c:17]3[c:18]2[n:19]1[CH2:20][...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN
null
null
C(Cl)(Cl)Cl.O.O1CCOCC1
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]
70.3
[{"value": 70.3, "product": "NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
Hydrogen chloride (100 mL of a 4 M solution in 1,4-dioxane) was added to tert-butyl[4-(4-amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)butyl]carbamate (10.0 g, 20.3 mmol), and the reaction was stirred for one hour. The reaction was adjusted to pH 11 with the addition of sodium hydroxide pellets in a small...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2c(c1)ncc1[nH]cnc12
HO-
C(Cl)(Cl)Cl.O.O1CCOCC1
null
1
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)OC(C)(C)C>C(Cl)(Cl)Cl.O.O1CCOCC1>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2e45af154c4a434dbd1369dfd3e515cd
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.CS(=O)(=O)Cl>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNS(C)(=O)=O
[OH-].[Na+].CS(=O)(=O)Cl.NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC.C(C)N(CC)CC>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNS(=O)(=O)C)COCC)Br
[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:17]3[c:18]2[n:19]1[CH2:20][CH2:21][CH2:22][CH2:23][NH2:24].Cl[S:25]([CH3:26])(=[O:27])=[O:28]>>[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:17]3[c:...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.CS(=O)(=O)Cl
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNS(C)(=O)=O
null
null
C(Cl)(Cl)Cl.O
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
c1ccc2c(c1)ncc1nc[nH]c12
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]
120.6
[{"value": 120.6, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNS(=O)(=O)C)COCC)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
Methanesulfonyl chloride (0.44 mL, 5.7 mmol) was added to a suspension of 1-(4-aminobutyl)-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-4-amine (2.04 g, 5.2 mmol) and triethylamine (0.94 mL, 6.8 mmol) in chloroform (100 mL), and the reaction was stirred for four hours. Water was added; a precipitate formed. The aqu...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2c(c1)ncc1[nH]cnc12
HCl
C(Cl)(Cl)Cl.O
null
4
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.CS(=O)(=O)Cl>C(Cl)(Cl)Cl.O>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0094d8a37a7a4e47843d835197d1b45e
CC(C)N=C=O.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)NC(C)C
NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC.C(C)(C)N=C=O>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(=O)NC(C)C)COCC)Br
[C:25](=[O:26])=[N:27][CH:28]([CH3:29])[CH3:30].[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:17]3[c:18]2[n:19]1[CH2:20][CH2:21][CH2:22][CH2:23][NH2:24]>>[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:...
CC(C)N=C=O.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)NC(C)C
null
null
C(Cl)(Cl)Cl
Acylation
Urea synthesis via isocyanate and primary amine
d39cd7dc52a79bb265ff8ef61ef7bf9dc7f7b5fb0150fcb4881bdfb18ab9c380
a5dc801930c765d2a435a0a2973e50163c305ba8e7641d6adbcc1550b7b96de7
c1ccc2c(c1)ncc1nc[nH]c12
[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]
76.4
[{"value": 76.4, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(=O)NC(C)C)COCC)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
45
MINUTE
A solution of 1-(4-aminobutyl)-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-4-amine (2.00 g, 5.1 mmol) in chloroform (36 mL) was cooled to 0° C., and a cold solution of isopropyl isocyanate (0.50 mL, 5.4 mmol) in chloroform (4 mL) was added slowly. A precipitate formed, and the reaction was stirred for 45 minutes. ...
10.6084/m9.figshare.5104873.v1
null
Isocyanate.Primary amine
Urea
null
null
c1ccc2c(c1)ncc1[nH]cnc12
null
C(Cl)(Cl)Cl
null
0.75
CC(C)N=C=O.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)NC(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-99bd2886c8094accacefd852ba8f9685
CC(C)C(=O)Cl.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCNCC1>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)CC(C)C)CC1
C(C)(=O)OCC.Cl.Cl.BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC3CCNCC3)COCC.C(C)N(CC)CC.C(C(C)C)(=O)Cl>>BrC=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC3CCN(CC3)C(=O)CC(C)C)COCC
Cl[C:27](=[O:26])[CH:28]([CH3:29])[CH3:30].[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:17]3[c:18]2[n:19]1[CH2:20][CH:21]1[CH2:22][CH2:23][NH:24][CH2:31][CH2:32]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]([Br:14])...
CC(C)C(=O)Cl.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCNCC1
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)CC(C)C)CC1
null
null
C(Cl)(Cl)Cl
Acylation
OtherReaction
aaa7c80569e6aa145ac8d7318e06893ee71aff0c965e85eca836522c948938d5
96cb0a2fed10552c5770a45a2d6523b47ac3e38928b4a9c698d8577451182dcd
c1ccc2c(c1)ncc1ncn(CC3CCNCC3)c12
Cl-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3](-[C;D1;H3:4])-[C;D1;H3:5].[C:6]-[C:7]-[NH;D2;+0:8]-[C:9]-[C:10]>>[C:6]-[C:7]-[N;H0;D3;+0:8](-[C:11](=[O;H0;D1;+0:2])-[CH2;D2;+0:1]-[C:3](-[C;D1;H3:4])-[C;D1;H3:5])-[C:9]-[C:10]
null
[]
null
null
1
HOUR
A solution of 7-bromo-2-ethoxymethyl-1-(piperidin-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-4-amine dihydrochloride (4.0 g, 8.1 mmol) and triethylamine (5.67 mL, 40.7 mmol) in chloroform (300 mL) was treated with isobutyryl chloride (0.85 mL, 8.1 mmol) according to the method described in Part A of Examples 583–611. The re...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Secondary amine
Tertiary amide
C1CCNCC1
C1CC[NH]CC1
c1ccc2c(c1)ncc1[nH]cnc12.C1CC[NH]CC1
null
C(Cl)(Cl)Cl
null
1
CC(C)C(=O)Cl.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCNCC1>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC1CCN(C(=O)CC(C)C)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dc51e2ec186444cea2088f7c0632f2df
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.O=C(Cl)C1CCCC1>>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)C1CCCC1
C1(CCCC1)C(=O)Cl.C1(CCCC1)C(=O)Cl.NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)COCC.C(C)N(CC)CC>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(=O)C2CCCC2)COCC)Br
[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:17]3[c:18]2[n:19]1[CH2:20][CH2:21][CH2:22][CH2:23][NH2:24].Cl[C:25](=[O:26])[CH:27]1[CH2:28][CH2:29][CH2:30][CH2:31]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]([Br:14])...
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.O=C(Cl)C1CCCC1
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)C1CCCC1
null
null
C(Cl)(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
O=C(NCCCCn1cnc2cnc3ccccc3c21)C1CCCC1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5]
64.2
[{"value": 64.2, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNC(=O)C2CCCC2)COCC)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2.5
HOUR
Cyclopentanecarbonyl chloride (0.80 mL, 6.6 mmol) was added dropwise over a period of five minutes to a suspension of 1-(4-aminobutyl)-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-4-amine (2.00 g, 5.1 mmol) and triethylamine (0.78 mL, 5.6 mmol) in chloroform (200 mL). The reaction was stirred for 2.5 hours and then...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2c(c1)ncc1[nH]cnc12.C1CCCC1
HCl
C(Cl)(Cl)Cl
null
2.5
CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.O=C(Cl)C1CCCC1>C(Cl)(Cl)Cl>CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNC(=O)C1CCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a6d64d1788c245cd93ee5ac0dfe8896d
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.CS(=O)(=O)Cl>>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNS(C)(=O)=O
NCCCCN1C(=NC=2C(=NC=3C=C(C=CC3C21)Br)N)CCC.C(C)N(CC)CC.CS(=O)(=O)Cl.C(C)N(CC)CC.CS(=O)(=O)Cl>>NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNS(=O)(=O)C)CCC)Br
[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]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[CH2:19][CH2:20][CH2:21][CH2:22][NH2:23].Cl[S:24]([CH3:25])(=[O:26])=[O:27]>>[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]([Br:13])[cH:14][cH:15][c:16]3[c:17]2[n:18]1[...
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.CS(=O)(=O)Cl
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNS(C)(=O)=O
null
null
C(Cl)(Cl)Cl
Miscellaneous
Sulfonamide synthesis (Schotten-Baumann) primary amine
a86b0632821e188c0a5dc5a5a2aac298ab3eccaee8a52ba46078c3d5975a290d
50f8fbf3d327483c3eeff8f6cbd4065e4c7600bb501fbe08958a5c79a0926428
c1ccc2c(c1)ncc1nc[nH]c12
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]
37.4
[{"value": 37.4, "product": "NC1=NC=2C=C(C=CC2C2=C1N=C(N2CCCCNS(=O)(=O)C)CCC)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
A suspension of 1-(4-aminobutyl)-7-bromo-2-propyl-1H-imidazo[4,5-c]quinolin-4-amine (3.27 g, 8.7 mmol) and triethylamine (3.82 mL, 11.3 mmol) in chloroform (165 mL) was cooled to 0° C. A cold solution of methanesulfonyl chloride (1.37 mL, 9.6 mmol) in chloroform (10 mL) was slowly added. The reaction was allowed to war...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2c(c1)ncc1[nH]cnc12
HCl
C(Cl)(Cl)Cl
0
null
CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCN.CS(=O)(=O)Cl>C(Cl)(Cl)Cl>CCCc1nc2c(N)nc3cc(Br)ccc3c2n1CCCCNS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dda085bf850b4d2b8343c992ca684d49
CC(C)(C)OC(=O)NCc1cccc(B(O)O)c1.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)(C)O>>CCOCc1nc2c(N)nc3cc(-c4cccc(CNC(=O)OC(C)(C)C)c4)ccc3c2n1CC(C)(C)O
NC1=NC=2C=C(C=CC2C2=C1N=C(N2CC(C)(O)C)COCC)Br.C(C)(C)(C)OC(=O)NCC=1C=C(C=CC1)B(O)O>>C(C)(C)(C)OC(NCC1=CC(=CC=C1)C=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)(C)O)COCC)=O
OB(O)[c:14]1[cH:15][cH:16][cH:17][c:18]([CH2:19][NH:20][C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27])[cH:28]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][O:3][CH2:2][CH3:1])[n:33]([CH2:34][C:35]([CH3:36])([CH3:37])[OH:38])[c:32]3[c:31]2[cH:30][cH:29]1>>[CH3:1][CH2:2][O:3][CH2:4][c:5]1[...
CC(C)(C)OC(=O)NCc1cccc(B(O)O)c1.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)(C)O
CCOCc1nc2c(N)nc3cc(-c4cccc(CNC(=O)OC(C)(C)C)c4)ccc3c2n1CC(C)(C)O
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
C1(=CC=CC=C1)C
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]
84.8
[{"value": 84.8, "product": "C(C)(C)(C)OC(NCC1=CC(=CC=C1)C=1C=CC=2C3=C(C(=NC2C1)N)N=C(N3CC(C)(C)O)COCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
1-(4-Amino-7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)-2-methylpropan-2-ol (2.62 g, 6.67 mmol) and 3-(N-tert-butoxycarbonylaminomethyl)phenylboronic acid (2.0 g, 8.0 mmol) were coupled according to the procedure described in Part J of Example 1. Palladium (II) acetate was added as a 5 mg/mL solution in tolue...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccc2c(c1)ncc1[nH]cnc12
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
c1ccc2c(c1)ncc1[nH]cnc12.c1ccccc1
HBr.B
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)C
null
null
CC(C)(C)OC(=O)NCc1cccc(B(O)O)c1.CCOCc1nc2c(N)nc3cc(Br)ccc3c2n1CC(C)(C)O>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)C>CCOCc1nc2c(N)nc3cc(-c4cccc(CNC(=O)OC(C)(C)C)c4)ccc3c2n1CC(C)(C)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f858daf9b78340f8a6c06509c19a3d65
C=CCCCCCC.CCCCCCCC[PH](=O)O>>CCCCCCCCP(=O)(O)CCCCCCCC
C(C1=CC=CC=C1)(=O)OOC(C1=CC=CC=C1)=O.C(C1=CC=CC=C1)(=O)OOC(C1=CC=CC=C1)=O.C(CCCCCCC)P(O)=O.C=CCCCCCC.C(C1=CC=CC=C1)(=O)OOC(C1=CC=CC=C1)=O>>C(CCCCCCC)P(O)(=O)CCCCCCCC
[CH2:12]=[CH:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][PH:9](=[O:10])[OH:11]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][P:9](=[O:10])([OH:11])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]
C=CCCCCCC.CCCCCCCC[PH](=O)O
CCCCCCCCP(=O)(O)CCCCCCCC
null
null
C(C)O
Miscellaneous
OtherReaction
57a64b6b42d462fe8276aa79a48b5b98ebab75830adad1905b3795c71ea65b06
b53d8f361e43dc967c3023dcafe218466acf623d0cf729a1557a2a80217926eb
null
[C:1]-[C:2]-[CH;D2;+0:3]=[CH2;D1;+0:4].[C:5]-[C:6]-[PH;D3;+0:7](=[O;D1;H0:8])-[O;D1;H1:9]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[P;H0;D4;+0:7](=[O;D1;H0:8])(-[O;D1;H1:9])-[C:6]-[C:5]
48.4
[{"value": 48.4, "product": "C(CCCCCCC)P(O)(=O)CCCCCCCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 32.8, "product": "C(CCCCCCC)P(O)(=O)CCCCCCCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a stirred mixture of 46.5 g (0.261 mol) of n-octylphosphinic acid in 250 mL 95% ethanol, 1-octene (58.6 g, 0.5218 mol) was added followed by 9.042 g (0.026 mol) of 70% benzoyl peroxide. The resulting mixture was refluxed for 8 hs, and then another 6.758 g (0.0196 mol) of benzoyl peroxide was added and the reaction c...
10.6084/m9.figshare.5104873.v1
null
Allyl
null
null
null
null
null
C(C)O
null
null
C=CCCCCCC.CCCCCCCC[PH](=O)O>C(C)O>CCCCCCCCP(=O)(O)CCCCCCCC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2a9a67b66c664cd1a09355b567f720a0
C=CCCCCCC.O=[PH2][O-]>>CCCCCCCC[PH](=O)O
OO.O.[PH2](=O)[O-].[Na+].C=CCCCCCC.OO>>C(CCCCCCC)P(O)=O
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH:7]=[CH2:8].[PH2:9](=[O:10])[O-:11]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][PH:9](=[O:10])[OH:11]
C=CCCCCCC.O=[PH2][O-]
CCCCCCCC[PH](=O)O
null
null
S(O)(O)(=O)=O.C(C)O
Miscellaneous
OtherReaction
57a64b6b42d462fe8276aa79a48b5b98ebab75830adad1905b3795c71ea65b06
b53d8f361e43dc967c3023dcafe218466acf623d0cf729a1557a2a80217926eb
null
[C:1]-[C:2]-[CH;D2;+0:3]=[CH2;D1;+0:4].[O-;H0;D1:5]-[PH2;D2;+0:6]=[O;D1;H0:7]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[PH;D3;+0:6](=[O;D1;H0:7])-[OH;D1;+0:5]
84.8
[{"value": 84.8, "product": "C(CCCCCCC)P(O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.8, "product": "C(CCCCCCC)P(O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a mixture of 95.1 g (0.897 mol) of sodium hypophosphite hydrate in 600 mL 95% ethanol, 23.8 mL of concentrated sulfuric acid was added. 1-Octene (33.6 g, 0.299 mol) was added to the stirred mixture followed by 1.69 g (0.0149 mol) of 30% hydrogen peroxide. The resulting mixture was refluxed for 8 hs, and then another...
10.6084/m9.figshare.5104873.v1
null
Allyl
null
null
null
null
null
S(O)(O)(=O)=O.C(C)O
null
null
C=CCCCCCC.O=[PH2][O-]>S(O)(O)(=O)=O.C(C)O>CCCCCCCC[PH](=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-238025faf88247d8961dfc9c207d64dc
C=CCCCC.O=[PH2][O-]>>CCCCCC[PH](=O)O
OO.O.[PH2](=O)[O-].[Na+].C=CCCCC.OO>>C(CCCCC)P(O)=O
[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]=[CH2:6].[PH2:7](=[O:8])[O-:9]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][PH:7](=[O:8])[OH:9]
C=CCCCC.O=[PH2][O-]
CCCCCC[PH](=O)O
null
null
S(O)(O)(=O)=O.C(C)O
Miscellaneous
OtherReaction
57a64b6b42d462fe8276aa79a48b5b98ebab75830adad1905b3795c71ea65b06
b53d8f361e43dc967c3023dcafe218466acf623d0cf729a1557a2a80217926eb
null
[C:1]-[C:2]-[CH;D2;+0:3]=[CH2;D1;+0:4].[O-;H0;D1:5]-[PH2;D2;+0:6]=[O;D1;H0:7]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[CH2;D2;+0:4]-[PH;D3;+0:6](=[O;D1;H0:7])-[OH;D1;+0:5]
82.4
[{"value": 82.4, "product": "C(CCCCC)P(O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.1, "product": "C(CCCCC)P(O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a mixture of 95.2 g (0.898 mol) of sodium hypophosphite hydrate in 600 mL 95% ethanol, 23.8 mL of concentrated sulfuric acid was added. 1-hexene (25.2 g, 0.30 mol) was added to the stirred mixture followed by 1.76 g (0.0155 mol) of 30% hydrogen peroxide. The resulting mixture was refluxed for 8 hs, and then another ...
10.6084/m9.figshare.5104873.v1
null
Allyl
null
null
null
null
null
S(O)(O)(=O)=O.C(C)O
null
null
C=CCCCC.O=[PH2][O-]>S(O)(O)(=O)=O.C(C)O>CCCCCC[PH](=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3117c94e8c2e4eec9d869a0c62704a73
Nc1ccc(I)cc1.O=CO>>O=CNc1ccc(I)cc1
IC1=CC=C(N)C=C1.C(C)(=O)OC(C)=O.C(=O)O>>C1=CC(=CC=C1NC=O)I
[NH2:3][c:4]1[cH:5][cH:6][c:7]([I:8])[cH:9][cH:10]1.O[CH:2]=[O:1]>>[O:1]=[CH:2][NH:3][c:4]1[cH:5][cH:6][c:7]([I:8])[cH:9][cH:10]1
Nc1ccc(I)cc1.O=CO
O=CNc1ccc(I)cc1
null
null
C1CCOC1.O.C(C)(=O)OCC.C1(=CC=CC=C1)C
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
c1ccccc1
O-[CH;D2;+0:1]=[O;D1;H0:2].[NH2;D1;+0:3]-[c:4](:[c:5]):[c:6]>>[O;D1;H0:2]=[CH;D2;+0:1]-[NH;D2;+0:3]-[c:4](:[c:5]):[c:6]
99
[{"value": 98.0, "product": "C1=CC(=CC=C1NC=O)I", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.0, "product": "C1=CC(=CC=C1NC=O)I", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of 4-iodoaniline (30.0 g, 137 mmol) in 100 mL THF and 100 mL toluene, a solution of acetic anhydride (16.0 g, 157 mmol) and formic acid (10.8 g, 235 mmol) was slowly added from an addition funnel under argon atmosphere. The reaction mixture temperature was maintained below 15° C. during the addition. Afte...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1
HO-
C1CCOC1.O.C(C)(=O)OCC.C1(=CC=CC=C1)C
null
8
Nc1ccc(I)cc1.O=CO>C1CCOC1.O.C(C)(=O)OCC.C1(=CC=CC=C1)C>O=CNc1ccc(I)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-df37945b51904d399bb64ad4006d4aeb
Brc1ccccc1.CC1(C)CC(=O)OC1=O>>CC(C)(CC(=O)c1ccc(Br)cc1)C(=O)O
BrC1=CC=CC=C1.CC1(C(OC(C1)=O)=O)C.[Al]>>BrC1=CC=C(C=C1)C(CC(C(=O)O)(C)C)=O
[cH:7]1[cH:8][cH:9][c:10]([Br:11])[cH:12][cH:13]1.[CH3:1][C:2]1([CH3:3])[CH2:4][C:5](=[O:6])[O:16][C:14]1=[O:15]>>[CH3:1][C:2]([CH3:3])([CH2:4][C:5](=[O:6])[c:7]1[cH:8][cH:9][c:10]([Br:11])[cH:12][cH:13]1)[C:14](=[O:15])[OH:16]
Brc1ccccc1.CC1(C)CC(=O)OC1=O
CC(C)(CC(=O)c1ccc(Br)cc1)C(=O)O
null
null
ClC(C)Cl
C-C Coupling
OtherReaction
95de0079bfd4d0e2b70eac1863ad8bac063c1a1557f674f5eb3c0cde67534555
4836357c99dfeeac9d5083fedc379181a858ae45ac77bd85eb46e7e1a9df36f0
c1ccccc1
[O;D1;H0:1]=[C:2]1-[C:3]-[C:4]-[C;H0;D3;+0:5](=[O;D1;H0:6])-[O;H0;D2;+0:7]-1.[c:8]:[c:9]:[cH;D2;+0:10]:[c:11]:[c:12]>>[O;D1;H0:1]=[C:2](-[OH;D1;+0:7])-[C:3]-[C:4]-[C;H0;D3;+0:5](=[O;D1;H0:6])-[c;H0;D3;+0:10](:[c:9]:[c:8]):[c:11]:[c:12]
63
[{"value": 63.0, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)O)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.6, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)O)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a chilled solution (ice/water bath) of bromobenzene (7.71 g, 49.1 mmol) and 3,3-dimethyldihydro-2,5-furandione (5.99 g, 46.7 mmol) in dichloroethane (150 mL) was added aluminum trichworide (13.28 g, 99.58 mmol). The ice bath was removed and the reaction mixture was stirred at rt overnight. The mixture was again chil...
10.6084/m9.figshare.5104873.v1
null
Anhydride
Carboxylic acid.Ketone
c1ccccc1.C1CCOC1
c1ccccc1
c1ccccc1
null
ClC(C)Cl
null
8
Brc1ccccc1.CC1(C)CC(=O)OC1=O>ClC(C)Cl>CC(C)(CC(=O)c1ccc(Br)cc1)C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-23f3c547abd546cb9fb9967371831408
CC(C)(CC(=O)c1ccc(Br)cc1)C(=O)O.COC(C)(C)OC>>COC(=O)C(C)(C)CC(=O)c1ccc(Br)cc1
BrC1=CC=C(C=C1)C(CC(C(=O)O)(C)C)=O.COC(C)(C)OC.Cl>>BrC1=CC=C(C=C1)C(CC(C(=O)OC)(C)C)=O
[OH:2][C:3](=[O:4])[C:5]([CH3:6])([CH3:7])[CH2:8][C:9](=[O:10])[c:11]1[cH:12][cH:13][c:14]([Br:15])[cH:16][cH:17]1.COC(C)(C)O[CH3:1]>>[CH3:1][O:2][C:3](=[O:4])[C:5]([CH3:6])([CH3:7])[CH2:8][C:9](=[O:10])[c:11]1[cH:12][cH:13][c:14]([Br:15])[cH:16][cH:17]1
CC(C)(CC(=O)c1ccc(Br)cc1)C(=O)O.COC(C)(C)OC
COC(=O)C(C)(C)CC(=O)c1ccc(Br)cc1
null
null
CO.O1CCOCC1
Heteroatom Alkylation and Arylation
O-methylation
996ec4961b01515261a54c290b3ca2791e1cd44e68716f1a7d216a92013249dc
f1d0c21bce3f84df8e09e027f5fecc48c78a31aaf69561ba0dce25419b3c823e
c1ccccc1
C-O-C(-C)(-C)-O-[CH3;D1;+0:1].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
99
[{"value": 99.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
50
CELSIUS
22
HOUR
To a solution of 4-(4-bromophenyl)-2,2-dimethyl-4-oxobutanoic acid (8.33 g, 29.2 mmol) and 2,2-dimethoxypropane (3.95 g, 37.9 mmol) in methanol (100 mL) was added 1 M HCl in dioxane (2.0 mL). The reaction mixture was stirred at 50° C. for 22 h. The mixture was concentrated under reduced pressure. Toluene (2×60 mL) was ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ether.Ether
Ester
null
null
c1ccccc1
HO-
CO.O1CCOCC1
50
22
CC(C)(CC(=O)c1ccc(Br)cc1)C(=O)O.COC(C)(C)OC>CO.O1CCOCC1>COC(=O)C(C)(C)CC(=O)c1ccc(Br)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e6285f699f614666a2681ea062cf0d89
COC(=O)C(C)(C)CC(=O)c1ccc(Br)cc1.O=CNc1ccc(I)cc1>>COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(NC=O)cc2)cc1
C1=CC(=CC=C1NC=O)I.B1(OC(C(O1)(C)C)(C)C)B2OC(C(O2)(C)C)(C)C.C(C)(=O)[O-].[K+].BrC1=CC=C(C=C1)C(CC(C(=O)OC)(C)C)=O.C([O-])([O-])=O.[Cs+].[Cs+]>>C(=O)NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OC)(C)C)=O
Br[c:14]1[cH:13][cH:12][c:11]([C:9]([CH2:8][C:5]([C:3]([O:2][CH3:1])=[O:4])([CH3:6])[CH3:7])=[O:10])[cH:25][cH:24]1.I[c:15]1[cH:16][cH:17][c:18]([NH:19][CH:20]=[O:21])[cH:22][cH:23]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]([CH3:6])([CH3:7])[CH2:8][C:9](=[O:10])[c:11]1[cH:12][cH:13][c:14](-[c:15]2[cH:16][cH:17][c:18]([NH:19][CH...
COC(=O)C(C)(C)CC(=O)c1ccc(Br)cc1.O=CNc1ccc(I)cc1
COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(NC=O)cc2)cc1
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
CN(C=O)C.O.C(C)(=O)OCC.CCCCCC
C-C Coupling
Negishi
c762f793fad28f910ecef7baabecb58fd3905901ac0af2c73542eba7e0faa33e
a7a4ce9a92e2f8a62d28956a69a5cc384426ab72416e87d68c6a3feb23c22d66
c1ccc(-c2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].I-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
68
[{"value": 68.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
To a 2-L three-necked round-bottomed flask were charged 4-iodoformanilide (30.0 g, 121 mmol, 1.0 eq), bis(pinacolato)diboron (30.8 g, 121 mmol, 1.0 eq), palladium acetate (0.82 g, 3.6 mmol, 3 mol %), potassium acetate (35.70 g, 364.3 mmol), and 500 mL N,N-dimethylformamide. The mixture was degassed by gently bubbling a...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
Br-.I-
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].CN(C=O)C.O.C(C)(=O)OCC.CCCCCC
80
null
COC(=O)C(C)(C)CC(=O)c1ccc(Br)cc1.O=CNc1ccc(I)cc1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].CN(C=O)C.O.C(C)(=O)OCC.CCCCCC>COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(NC=O)cc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-009a97990c0745b6937ef7f388424e8c
COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(NC=O)cc2)cc1>>COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(N)cc2)cc1
C(=O)NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OC)(C)C)=O.Cl>>NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OC)(C)C)=O
O=C[NH:19][c:18]1[cH:17][cH:16][c:15](-[c:14]2[cH:13][cH:12][c:11]([C:9]([CH2:8][C:5]([C:3]([O:2][CH3:1])=[O:4])([CH3:6])[CH3:7])=[O:10])[cH:23][cH:22]2)[cH:21][cH:20]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]([CH3:6])([CH3:7])[CH2:8][C:9](=[O:10])[c:11]1[cH:12][cH:13][c:14](-[c:15]2[cH:16][cH:17][c:18]([NH2:19])[cH:20][cH:21]2...
COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(NC=O)cc2)cc1
COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(N)cc2)cc1
null
null
CO
Reduction
Reduction of primary amides to amines
755df58c254dea764fdda078ffd678ec540bba057c83683be04c253f1270ac7b
025f7cefe51e71668ad5d09fca32df168e9b538347403e4d5c1748073e538adc
c1ccc(-c2ccccc2)cc1
O=C-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
95.4
[{"value": 95.0, "product": "NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OC)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.4, "product": "NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OC)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a suspension of methyl 4-[4′-(formylamino)-1,1′-biphenyl-4-yl]-2,2-dimethyl-4-oxobutanoate (2.40 g, 7.07 mmol) in 20 mL methanol, was added 7 mL concentrated hydrochloric acid at below rt. The reaction mixture was stirred at rt overnight. The mixture was concentrated under reduced pressure and saturated aqueous sodi...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
Primary amine
null
null
c1ccccc1.c1ccccc1
Other
CO
null
8
COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(NC=O)cc2)cc1>CO>COC(=O)C(C)(C)CC(=O)c1ccc(-c2ccc(N)cc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9ff66aac35af4237ad585c7ebc53e6dd
CCOC(=O)C(CCc1ccccc1)C(=O)OCC.O=C(CBr)c1ccc(Br)cc1>>CCOC(=O)C(CCc1ccccc1)(CC(=O)c1ccc(Br)cc1)C(=O)OCC
Cl.[H-].[Na+].BrCC(=O)C1=CC=C(C=C1)Br.C1(=CC=CC=C1)CCC(C(=O)OCC)C(=O)OCC>>BrC1=CC=C(C=C1)C(CC(C(=O)OCC)(C(=O)OCC)CCC1=CC=CC=C1)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)[C:25](=[O:26])[O:27][CH2:28][CH3:29].Br[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][c:21]([Br:22])[cH:23][cH:24]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)([CH2:15][C:1...
CCOC(=O)C(CCc1ccccc1)C(=O)OCC.O=C(CBr)c1ccc(Br)cc1
CCOC(=O)C(CCc1ccccc1)(CC(=O)c1ccc(Br)cc1)C(=O)OCC
null
null
O1CCCC1
C-C Coupling
OtherReaction
4bb1433a83171a818741815ed1611f54dc47d930932c002b83e8524407ba2582
d7a41d4d502746dc050b2738c9dd1b697535250fee467eca2d3c201fc4e0267b
O=C(CCCCc1ccccc1)c1ccccc1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[CH;D3;+0:9](-[C:10]-[C:11])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[C;H0;D4;+0:9](-[C:10]-[C:11])(-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]
61
[{"value": 61.0, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)OCC)(C(=O)OCC)CCC1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 60.5, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)OCC)(C(=O)OCC)CCC1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
16
HOUR
To a 500 mL 3-neck round-bottom flask equipped with an argon inlet and an addition funnel, was added sodium hydride (95%, 1.40 g, 58.3 mmol) followed by tetrahydrofuran (30 mL). The resulting suspension was then cooled to 0° C. and diethyl 2-(2-phenylethyl)malonate (14.0 g, 53.0 mmol) in tetrahydrofuran (20 mL) was add...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Ester.Ester
Ketone.Ester.Ester
null
null
c1ccccc1.c1ccccc1
HBr
O1CCCC1
0
16
CCOC(=O)C(CCc1ccccc1)C(=O)OCC.O=C(CBr)c1ccc(Br)cc1>O1CCCC1>CCOC(=O)C(CCc1ccccc1)(CC(=O)c1ccc(Br)cc1)C(=O)OCC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8fb6d4a6537a45d7bc04373d65cf36ce
CCOC(=O)C(CCc1ccccc1)(CC(=O)c1ccc(Br)cc1)C(=O)OCC>>CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(Br)cc1
BrC1=CC=C(C=C1)C(CC(C(=O)OCC)(C(=O)OCC)CCC1=CC=CC=C1)=O.[OH-].[Na+]>>BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O
CCOC(=O)[C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20][c:21]([Br:22])[cH:23][cH:24]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)[CH2:15][C:16](=[O:17])[c:18]1[cH:19][cH:20...
CCOC(=O)C(CCc1ccccc1)(CC(=O)c1ccc(Br)cc1)C(=O)OCC
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(Br)cc1
null
null
CC(=O)C.C(C)O
Reduction
OtherReaction
33f176f6ce02426b2726e71e3c19f64673952a2b50dd48518b89a08efe25965b
b45711df98eaf2a3f54e3027da3f1b57580ab2f6d54e9ac2a56731961e64969a
O=C(CCCCc1ccccc1)c1ccccc1
C-C-O-C(=O)-[C;H0;D4;+0:1](-[C:2]-[C:3](=[O;D1;H0:4])-[c:5])(-[C:6]-[C:7])-[C:8](=[O;D1;H0:9])-[#8:10]-[C:11]>>[C:11]-[#8:10]-[C:8](=[O;D1;H0:9])-[CH;D3;+0:1](-[C:2]-[C:3](=[O;D1;H0:4])-[c:5])-[C:6]-[C:7]
65
[{"value": 65.0, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 64.9, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
null
null
To a solution of diethyl 2-[2-(4-bromophenyl)-2-oxoethyl]-2-(2-phenylethyl)malonate (7.89 g, 17.1 mmol) in acetone (18.5 mL) and ethanol (17.0 mL) was added 1 N aqueous sodium hydroxide solution (17.1 mL), and the resulting solution was heated at 50° C. for 3 h. Solvent was then removed under reduced pressure via rotar...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Ester
null
null
c1ccccc1.c1ccccc1
HO-
CC(=O)C.C(C)O
50
null
CCOC(=O)C(CCc1ccccc1)(CC(=O)c1ccc(Br)cc1)C(=O)OCC>CC(=O)C.C(C)O>CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(Br)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-401204b21f9244dfb803dad51a9352ec
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(Br)cc1.O=[N+]([O-])c1ccc(B(O)O)cc1>>CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1
C1(=CC=CC=C1)C.C([O-])([O-])=O.[Na+].[Na+].BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O.[N+](=O)([O-])C1=CC=C(C=C1)B(O)O>>[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O
Br[c:21]1[cH:20][cH:19][c:18]([C:16]([CH2:15][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)=[O:17])[cH:32][cH:31]1.OB(O)[c:22]1[cH:23][cH:24][c:25]([N+:26](=[O:27])[O-:28])[cH:29][cH:30]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12]...
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(Br)cc1.O=[N+]([O-])c1ccc(B(O)O)cc1
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1
null
null
O1CCOCC1
C-C Coupling
Suzuki coupling with boronic acids
d79a78c79f0c392f0911481acf5c300cc98205269acdb93c24fb610a61c4c868
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C(CCCCc1ccccc1)c1ccc(-c2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
75.2
[{"value": 75.0, "product": "[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.2, "product": "[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
Ethyl 4-(4-bromophenyl)-4-oxo-2-(2-phenylethyl)butanoate (4.32 g, 11.1 mmol) and 4-nitrophenylboronic acid (2.22, 13.3 mmol) was added to a dry flask under argon. Toluene (100 mL), dioxane (25 mL), saturated aqueous sodium carbonate (30 mL), and [1,1′-bis(diphenyl-phosphino)-ferrocene]dichloro palladium(II) (1:1 comple...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1
HBr.B
O1CCOCC1
85
null
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(Br)cc1.O=[N+]([O-])c1ccc(B(O)O)cc1>O1CCOCC1>CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a3f07a1b4c274a639afd3ac301a7a5b5
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1>>CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc(N)cc2)cc1
[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O.Cl>>NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O
O=[N+:26]([O-])[c:25]1[cH:24][cH:23][c:22](-[c:21]2[cH:20][cH:19][c:18]([C:16]([CH2:15][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][CH2:8][c:9]3[cH:10][cH:11][cH:12][cH:13][cH:14]3)=[O:17])[cH:30][cH:29]2)[cH:28][cH:27]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1...
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc(N)cc2)cc1
null
[Fe]
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C(CCCCc1ccccc1)c1ccc(-c2ccccc2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
95.2
[{"value": 95.0, "product": "NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.2, "product": "NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of ethyl 4-(4′-nitro-1,1′-biphenyl-4-yl)-4-oxo-2-(2-phenylethyl)butanoate (5.35 g, 12.4 mmol) in 85% ethanol (160 mL) was added iron powder (6.94 g) followed by a 2 N aqueous solution of hydrochloric acid (6.2 mL). The resulting mixture was refluxed for 2.5 h, filtered through a pad of Celite®, and extrac...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccccc1.c1ccccc1
Other
[Fe].C(C)O
null
null
CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1>[Fe].C(C)O>CCOC(=O)C(CCc1ccccc1)CC(=O)c1ccc(-c2ccc(N)cc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ee9c0b103ab042eea52701b076134912
CC(C)=O.CCCC(CC(=O)c1ccc(Br)cc1)(C(=O)[O-])C(=O)[O-]>>CCCC(CC(=O)c1ccc(Br)cc1)C(=O)OCC
BrC1=CC=C(C=C1)C(CC(C(=O)[O-])(C(=O)[O-])CCC)=O.CC(=O)C.[OH-].[Na+]>>BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCC)=O
C[C:18](=[O:17])[CH3:19].O=C([O-])[C:4]([CH2:3][CH2:2][CH3:1])([CH2:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([Br:12])[cH:13][cH:14]1)[C:15]([O-])=[O:16]>>[CH3:1][CH2:2][CH2:3][CH:4]([CH2:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([Br:12])[cH:13][cH:14]1)[C:15](=[O:16])[O:17][CH2:18][CH3:19]
CC(C)=O.CCCC(CC(=O)c1ccc(Br)cc1)(C(=O)[O-])C(=O)[O-]
CCCC(CC(=O)c1ccc(Br)cc1)C(=O)OCC
null
null
C(C)O
Acylation
OtherReaction
ab932c02ad5f3de757fcd72006af4dfbbf5ed07dbd4c1d8e6c87cdb2a27d31ab
30c2c127c5cd46c77c59e05296c08e25077e8f68ec886ea7c29a791fdf58b61a
c1ccccc1
C-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;H0;D1;+0:3].O=C(-[O-])-[C;H0;D4;+0:4](-[C:5]-[C:6])(-[C:7]-[C:8](=[O;D1;H0:9])-[c:10])-[C;H0;D3;+0:11](-[O-])=[O;D1;H0:12]>>[C:6]-[C:5]-[CH;D3;+0:4](-[C:7]-[C:8](=[O;D1;H0:9])-[c:10])-[C;H0;D3;+0:11](=[O;D1;H0:12])-[O;H0;D2;+0:3]-[CH2;D2;+0:1]-[C;D1;H3:2]
20
[{"value": 20.0, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCC)=O", "details": "PERCENTYIELD", "is_desired": false}]
55
CELSIUS
15
MINUTE
To a 200 mL flask was added crude 2-[2-(4-bromophenyl)-2-oxoethyl]-2-propylmalonate (7.62 g, 19.2 mmol), acetone (21 mL), and ethanol (19 mL), followed by addition of 1 N aqueous sodium hydroxide solution (19.1 mL). The reaction mixture was heated to 55° C. for 3 h. The clear, orange-red reaction mixture was then conce...
10.6084/m9.figshare.5104873.v1
null
Ketone
Ester
null
null
c1ccccc1
Other
C(C)O
55
0.25
CC(C)=O.CCCC(CC(=O)c1ccc(Br)cc1)(C(=O)[O-])C(=O)[O-]>C(C)O>CCCC(CC(=O)c1ccc(Br)cc1)C(=O)OCC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a78d2dcb1e5548479df3ef45416b6e74
CCCC(CC(=O)c1ccc(Br)cc1)C(=O)OCC.O=[N+]([O-])c1ccc(B(O)O)cc1>>CCCC(CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1)C(=O)OCC
C([O-])([O-])=O.[Na+].[Na+].BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCC)=O.[N+](=O)([O-])C1=CC=C(C=C1)B(O)O>>[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC)=O
Br[c:11]1[cH:10][cH:9][c:8]([C:6]([CH2:5][CH:4]([CH2:3][CH2:2][CH3:1])[C:23](=[O:24])[O:25][CH2:26][CH3:27])=[O:7])[cH:22][cH:21]1.OB(O)[c:12]1[cH:13][cH:14][c:15]([N+:16](=[O:17])[O-:18])[cH:19][cH:20]1>>[CH3:1][CH2:2][CH2:3][CH:4]([CH2:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11](-[c:12]2[cH:13][cH:14][c:15]([N+:16](=[O:...
CCCC(CC(=O)c1ccc(Br)cc1)C(=O)OCC.O=[N+]([O-])c1ccc(B(O)O)cc1
CCCC(CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1)C(=O)OCC
null
null
O1CCOCC1.C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
d79a78c79f0c392f0911481acf5c300cc98205269acdb93c24fb610a61c4c868
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:8]:[c:7]:[c;H0;D3;+0:6](-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:9]:[c:10]
48
[{"value": 48.0, "product": "[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 46.9, "product": "[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC(C(=O)OCC)CCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
15
MINUTE
To a 150 mL 3-neck flask fitted with a reflux condenser was added ethyl 2-[2-(4-bromophenyl)-2-oxoethyl]pentanoate (1.33 g, 4.10 mmol) and 4-nitro phenyl boronic acid (0.81 g, 4.9 mmol), dissolved in toluene (37 mL) and dioxane (10 mL), followed by addition of saturated aqueous sodium carbonate (11 mL). A thin-gauge ne...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
HBr.B
O1CCOCC1.C1(=CC=CC=C1)C
85
0.25
CCCC(CC(=O)c1ccc(Br)cc1)C(=O)OCC.O=[N+]([O-])c1ccc(B(O)O)cc1>O1CCOCC1.C1(=CC=CC=C1)C>CCCC(CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1)C(=O)OCC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4d6fa58708e84e73b1226055e2995034
CCOC(=O)C(CCOC)(CC(=O)c1ccc(Br)cc1)C(=O)OCC>>CCOC(=O)C(CCOC)CC(=O)c1ccc(Br)cc1
[OH-].[Na+].BrC1=CC=C(C=C1)C(CC(C(=O)OCC)(C(=O)OCC)CCOC)=O>>BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCOC)=O
CCOC(=O)[C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH2:7][CH2:8][O:9][CH3:10])[CH2:11][C:12](=[O:13])[c:14]1[cH:15][cH:16][c:17]([Br:18])[cH:19][cH:20]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][CH2:8][O:9][CH3:10])[CH2:11][C:12](=[O:13])[c:14]1[cH:15][cH:16][c:17]([Br:18])[cH:19][cH:20]1
CCOC(=O)C(CCOC)(CC(=O)c1ccc(Br)cc1)C(=O)OCC
CCOC(=O)C(CCOC)CC(=O)c1ccc(Br)cc1
null
null
CC(=O)C.C(C)O
Reduction
OtherReaction
33f176f6ce02426b2726e71e3c19f64673952a2b50dd48518b89a08efe25965b
b45711df98eaf2a3f54e3027da3f1b57580ab2f6d54e9ac2a56731961e64969a
c1ccccc1
C-C-O-C(=O)-[C;H0;D4;+0:1](-[C:2]-[C:3](=[O;D1;H0:4])-[c:5])(-[C:6]-[C:7])-[C:8](=[O;D1;H0:9])-[#8:10]-[C:11]>>[C:11]-[#8:10]-[C:8](=[O;D1;H0:9])-[CH;D3;+0:1](-[C:2]-[C:3](=[O;D1;H0:4])-[c:5])-[C:6]-[C:7]
86
[{"value": 86.0, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCOC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.0, "product": "BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCOC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
55
CELSIUS
15
MINUTE
To a 150 mL flask was added diethyl 2-[2-(4-bromophenyl)-2-oxoethyl]-2-(2-methoxyethyl)malonate (1.59 g, 3.59 mmol) dissolved in acetone (16 mL) and ethanol (16 mL), followed by addition of 1N aqueous sodium hydroxide solution (3.6 mL). The reaction mixture was then heated at 55° C. for 3 h. The reaction mixture was co...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Ester
null
null
c1ccccc1
HO-
CC(=O)C.C(C)O
55
0.25
CCOC(=O)C(CCOC)(CC(=O)c1ccc(Br)cc1)C(=O)OCC>CC(=O)C.C(C)O>CCOC(=O)C(CCOC)CC(=O)c1ccc(Br)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5dcca08f75f24c8a9f19bca88699582c
CCOC(=O)C(CCOC)CC(=O)c1ccc(Br)cc1.O=[N+]([O-])c1ccc(B(O)O)cc1>>CCOC(=O)C(CCOC)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1
C([O-])([O-])=O.[Na+].[Na+].BrC1=CC=C(C=C1)C(CC(C(=O)OCC)CCOC)=O.[N+](=O)([O-])C1=CC=C(C=C1)B(O)O>>COCCC(C(=O)OCC)CC(=O)C1=CC=C(C=C1)C1=CC=C(C=C1)[N+](=O)[O-]
Br[c:17]1[cH:16][cH:15][c:14]([C:12]([CH2:11][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][CH2:8][O:9][CH3:10])=[O:13])[cH:28][cH:27]1.OB(O)[c:18]1[cH:19][cH:20][c:21]([N+:22](=[O:23])[O-:24])[cH:25][cH:26]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][CH2:8][O:9][CH3:10])[CH2:11][C:12](=[O:13])[c:14]1[cH:15][cH:1...
CCOC(=O)C(CCOC)CC(=O)c1ccc(Br)cc1.O=[N+]([O-])c1ccc(B(O)O)cc1
CCOC(=O)C(CCOC)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1
null
null
O1CCOCC1.C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
d79a78c79f0c392f0911481acf5c300cc98205269acdb93c24fb610a61c4c868
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
88
[{"value": 88.0, "product": "COCCC(C(=O)OCC)CC(=O)C1=CC=C(C=C1)C1=CC=C(C=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.3, "product": "COCCC(C(=O)OCC)CC(=O)C1=CC=C(C=C1)C1=CC=C(C=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
15
MINUTE
To a 150 mL 3-neck flask fitted with a reflux condenser was added ethyl 4-(4-bromophenyl)-2-(2-methoxyethyl)-4-oxobutanoate (1.06 g, 3.09 mmol) and 4-nitro-phenyl boronic acid (0.62 g, 3.70 mmol) dissolved in toluene (30 mL) and dioxane (8.50 mL), followed by addition of saturated aqueous sodium carbonate solution (8.5...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
HBr.B
O1CCOCC1.C1(=CC=CC=C1)C
85
0.25
CCOC(=O)C(CCOC)CC(=O)c1ccc(Br)cc1.O=[N+]([O-])c1ccc(B(O)O)cc1>O1CCOCC1.C1(=CC=CC=C1)C>CCOC(=O)C(CCOC)CC(=O)c1ccc(-c2ccc([N+](=O)[O-])cc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b2b04ebbc53f4f219f2866ba91f72edb
COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCCC1.O=[N+]([O-])c1ccc(B(O)O)cc1>>COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCCC1
C([O-])([O-])=O.[Na+].[Na+].BrC1=CC=C(C=C1)C(CC1(CCCC1)C(=O)OC)=O.[N+](=O)([O-])C1=CC=C(C=C1)B(O)O.C1(=CC=CC=C1)C>>[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCCC1)C(=O)OC)=O
Br[c:12]1[cH:11][cH:10][c:9]([C:7]([CH2:6][C:5]2([C:3]([O:2][CH3:1])=[O:4])[CH2:24][CH2:25][CH2:26][CH2:27]2)=[O:8])[cH:23][cH:22]1.OB(O)[c:13]1[cH:14][cH:15][c:16]([N+:17](=[O:18])[O-:19])[cH:20][cH:21]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][C:7](=[O:8])[c:9]2[cH:10][cH:11][c:12](-[c:13]3[cH:14][cH:15][c:16]([N+:17...
COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCCC1.O=[N+]([O-])c1ccc(B(O)O)cc1
COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCCC1
null
null
O1CCOCC1.C(C)(=O)OCC.[Cl-].[Na+]
C-C Coupling
Suzuki coupling with boronic acids
d79a78c79f0c392f0911481acf5c300cc98205269acdb93c24fb610a61c4c868
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C(CC1CCCC1)c1ccc(-c2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
96.8
[{"value": 93.0, "product": "[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCCC1)C(=O)OC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.8, "product": "[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCCC1)C(=O)OC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
15
MINUTE
To a 150 mL 3-neck flask fitted with a reflux condenser was added methyl 1-[2-(4-bromophenyl)-2-oxoethyl]cyclopentanecarboxylate (1.58 g, 4.64 mmol), 4-nitro phenyl boronic acid (0.93 g, 5.6 mmol), toluene (45 mL), and dioxane (13 mL), followed by the addition of a saturated aqueous sodium carbonate solution (13 mL). T...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.C1CCCC1
HBr.B
O1CCOCC1.C(C)(=O)OCC.[Cl-].[Na+]
85
0.25
COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCCC1.O=[N+]([O-])c1ccc(B(O)O)cc1>O1CCOCC1.C(C)(=O)OCC.[Cl-].[Na+]>COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e3ba7497cd344fb1b0003b2107debd6a
COS(=O)(=O)OC.O=C(O)C1CCOCC1>>COC(=O)C1CCOCC1
O1CCC(CC1)C(=O)O.C([O-])([O-])=O.[K+].[K+].S(=O)(=O)(OC)OC>>O1CCC(CC1)C(=O)OC
COS(=O)(=O)O[CH3:1].[OH:2][C:3](=[O:4])[CH:5]1[CH2:6][CH2:7][O:8][CH2:9][CH2:10]1>>[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:6][CH2:7][O:8][CH2:9][CH2:10]1
COS(=O)(=O)OC.O=C(O)C1CCOCC1
COC(=O)C1CCOCC1
null
null
CC(=O)C
Heteroatom Alkylation and Arylation
Methylation of OH with DMS
9474aa79a2adc7353c0c02444ca598a6f486ecdd7ed5edb9ae0645721ee50389
badd4f82161bb0ee7acffd023ea4caae5d036bce7065c10ab0a06e83a6a6f119
C1CCOCC1
C-O-S(=O)(=O)-O-[CH3;D1;+0:1].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
99.3
[{"value": 99.0, "product": "O1CCC(CC1)C(=O)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.3, "product": "O1CCC(CC1)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Tetrahydro-2H-pyran-4-carboxylic acid (1.00 g, 7.68 mmol) was slowly added to a stirred suspension of anhydrous potassium carbonate (1.17 g, 8.45 mmol) in acetone (40 mL), followed by dimethyl sulfate (0.8 mL, 8.45 mmol). The mixture was stirred and heated for 3 h. The inorganic salts were then removed by filtration an...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ester
null
null
C1CCOCC1
HO-
CC(=O)C
null
null
COS(=O)(=O)OC.O=C(O)C1CCOCC1>CC(=O)C>COC(=O)C1CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d5977edb28e5424eb7a5537df973da53
CC(C)(C)OC(=O)CBr.COC(=O)C1CCOCC1>>COC(=O)C1(CC(=O)OC(C)(C)C)CCOCC1
BrCC(=O)OC(C)(C)C.C(CCC)[Li].C(C)(C)NC(C)C.O1CCC(CC1)C(=O)OC>>C(C)(C)(C)OC(CC1(CCOCC1)C(=O)OC)=O
Br[CH2:6][C:7](=[O:8])[O:9][C:10]([CH3:11])([CH3:12])[CH3:13].[CH3:1][O:2][C:3](=[O:4])[CH:5]1[CH2:14][CH2:15][O:16][CH2:17][CH2:18]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][C:7](=[O:8])[O:9][C:10]([CH3:11])([CH3:12])[CH3:13])[CH2:14][CH2:15][O:16][CH2:17][CH2:18]1
CC(C)(C)OC(=O)CBr.COC(=O)C1CCOCC1
COC(=O)C1(CC(=O)OC(C)(C)C)CCOCC1
null
null
O.O1CCCC1
C-C Coupling
OtherReaction
f1ac808bca1710c7bfd2d73523f305c1160f7ea189fea2b67137f9fc598cd703
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
C1CCOCC1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5](-[C;D1;H3:6])(-[C;D1;H3:7])-[C;D1;H3:8].[C;D1;H3:9]-[#8:10]-[C:11](=[O;D1;H0:12])-[CH;D3;+0:13]1-[C:14]-[C:15]-[#8:16]-[C:17]-[C:18]-1>>[C;D1;H3:6]-[C:5](-[C;D1;H3:7])(-[C;D1;H3:8])-[#8:4]-[C:2](=[O;D1;H0:3])-[CH2;D2;+0:1]-[C;H0;D4;+0:13]1(-[C:11](=[O;D1;H0:12])-[#8:10]...
56.8
[{"value": 56.0, "product": "C(C)(C)(C)OC(CC1(CCOCC1)C(=O)OC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 56.8, "product": "C(C)(C)(C)OC(CC1(CCOCC1)C(=O)OC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-35
CELSIUS
1
HOUR
Diisopropylamine (1.28 mL, 9.16 mmol) was diluted with tetrahydrofuran (2 mL) and cooled to −78° C. n-Butyllithium (2.5 M, 3.66 mL, 9.16 mmol) was added dropwise, and the solution was allowed to stir for 1 h. Methyl tetrahydro-2H-pyran-4-carboxylate (1.1 g, 7.63 mmol) was added as a solution in tetrahydrofuran (1.5 mL)...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
C1CCOCC1
C1CCOCC1
C1CCOCC1
HBr
O.O1CCCC1
-35
1
CC(C)(C)OC(=O)CBr.COC(=O)C1CCOCC1>O.O1CCCC1>COC(=O)C1(CC(=O)OC(C)(C)C)CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-32f0b45fdb2849eb997c167048a03d3c
COC(=O)C1(CC(=O)OC(C)(C)C)CCOCC1>>COC(=O)C1(CC(=O)O)CCOCC1
C(C)(C)(C)OC(CC1(CCOCC1)C(=O)OC)=O.FC(C(=O)O)(F)F>>COC(=O)C1(CCOCC1)CC(=O)O
CC(C)(C)[O:9][C:7]([CH2:6][C:5]1([C:3]([O:2][CH3:1])=[O:4])[CH2:10][CH2:11][O:12][CH2:13][CH2:14]1)=[O:8]>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][C:7](=[O:8])[OH:9])[CH2:10][CH2:11][O:12][CH2:13][CH2:14]1
COC(=O)C1(CC(=O)OC(C)(C)C)CCOCC1
COC(=O)C1(CC(=O)O)CCOCC1
null
null
ClCCl
Deprotection
Deprotection of carboxylic acid
152e5537e48c95b4a3e767536b0f9f68d1308e5f484070828ab5ed951805157a
7f019d4cfe9b3036d0a2d3a3209aa0e1fcb05418ebee15a4be5e125d315d5f01
C1CCOCC1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
104.5
[{"value": 94.0, "product": "COC(=O)C1(CCOCC1)CC(=O)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 104.5, "product": "COC(=O)C1(CCOCC1)CC(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
To a solution of methyl 4-(2-tert-butoxy-2-oxoethyl)tetrahydro-2H-pyran-4-carboxylate (1.1 g, 4.26 mmol) in dichloromethane (5.0 mL) was added trifluoroacetic acid (5.0 mL) and the resulting solution was stirred at rt for 5 h. The mixture was concentrated under reduced pressure to afford [4-(methoxycarbonyl)tetrahydro-...
10.6084/m9.figshare.5104873.v1
null
Ester.Boc
Carboxylic acid
null
null
C1CCOCC1
Other
ClCCl
null
5
COC(=O)C1(CC(=O)OC(C)(C)C)CCOCC1>ClCCl>COC(=O)C1(CC(=O)O)CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2886457481ea407a9836e9cd75ae21a7
Brc1ccccc1.COC(=O)C1(CC(=O)Cl)CCOCC1>>COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCOCC1
ClC(CC1(CCOCC1)C(=O)OC)=O.BrC1=CC=CC=C1.[Cl-].[Al+3].[Cl-].[Cl-]>>BrC1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O
[cH:9]1[cH:10][cH:11][c:12]([Br:13])[cH:14][cH:15]1.Cl[C:7]([CH2:6][C:5]1([C:3]([O:2][CH3:1])=[O:4])[CH2:16][CH2:17][O:18][CH2:19][CH2:20]1)=[O:8]>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][C:7](=[O:8])[c:9]2[cH:10][cH:11][c:12]([Br:13])[cH:14][cH:15]2)[CH2:16][CH2:17][O:18][CH2:19][CH2:20]1
Brc1ccccc1.COC(=O)C1(CC(=O)Cl)CCOCC1
COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCOCC1
null
null
ClCCl
C-C Coupling
Friedel-Crafts acylation
55541449ad4f182ef3dc0497085b282b1dcb76e0fb5ed140dc4eab4973eacb28
fe2a4a0dfbb5b71b9a065e092364c64b22b4eb1ad4d6ba2a1e8edc9d31fce3e4
O=C(CC1CCOCC1)c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]-[C:5](-[#8:6])=[O;D1;H0:7].[c:8]:[c:9]:[cH;D2;+0:10]:[c:11]:[c:12]>>[#8:6]-[C:5](=[O;D1;H0:7])-[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:10](:[c:9]:[c:8]):[c:11]:[c:12]
55
[{"value": 55.0, "product": "BrC1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 55.0, "product": "BrC1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a solution of methyl 4-(2-chloro-2-oxoethyl)tetrahydro-2H-pyran-4-carboxylate (1.06 g, 4.8 mmol) and bromobenzene (1.13 g, 7.21 mmol) in dichloromethane (20 mL) at 0° C. was added aluminum chloride (1.92 g, 14.4 mmol). The ice-water bath was removed and the reaction mixture was stirred at rt for 16 h. The mixture wa...
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Ketone
c1ccccc1
c1ccccc1
c1ccccc1.C1CCOCC1
HCl
ClCCl
null
16
Brc1ccccc1.COC(=O)C1(CC(=O)Cl)CCOCC1>ClCCl>COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-95ac54c9a77a48bb970bfef33b2bcba5
COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCOCC1.O=[N+]([O-])c1ccc(B(O)O)cc1>>COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCOCC1
BrC1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O.[N+](=O)([O-])C1=CC=C(C=C1)B(O)O.C([O-])([O-])=O.[Na+].[Na+].ClCCl>>[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O
Br[c:12]1[cH:11][cH:10][c:9]([C:7]([CH2:6][C:5]2([C:3]([O:2][CH3:1])=[O:4])[CH2:24][CH2:25][O:26][CH2:27][CH2:28]2)=[O:8])[cH:23][cH:22]1.OB(O)[c:13]1[cH:14][cH:15][c:16]([N+:17](=[O:18])[O-:19])[cH:20][cH:21]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][C:7](=[O:8])[c:9]2[cH:10][cH:11][c:12](-[c:13]3[cH:14][cH:15][c:16](...
COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCOCC1.O=[N+]([O-])c1ccc(B(O)O)cc1
COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCOCC1
null
C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2]
O.O1CCOCC1.C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
d79a78c79f0c392f0911481acf5c300cc98205269acdb93c24fb610a61c4c868
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C(CC1CCOCC1)c1ccc(-c2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
79.3
[{"value": 79.0, "product": "[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.3, "product": "[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
Methyl 4-[2-(4-bromophenyl)-2-oxoethyl]tetrahydro-2H-pyran-4-carboxylate (820 mg, 2.40 mmol) and 4-nitrophenyl boronic acid (481 mg, 2.88 mmol) were combined in a dry flask under argon. Toluene (20 mL) and dioxane (5 mL) were added, and the resulting solution was degassed for 30 minutes by a flow of argon. The degassin...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.C1CCOCC1
HBr.B
C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].O.O1CCOCC1.C1(=CC=CC=C1)C
85
null
COC(=O)C1(CC(=O)c2ccc(Br)cc2)CCOCC1.O=[N+]([O-])c1ccc(B(O)O)cc1>C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].O.O1CCOCC1.C1(=CC=CC=C1)C>COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ffffb01d3bdd4e01bba1881b67a7067c
COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCOCC1>>COC(=O)C1(CC(=O)c2ccc(-c3ccc(N)cc3)cc2)CCOCC1
[N+](=O)([O-])C1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O.Cl>>NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O
O=[N+:17]([O-])[c:16]1[cH:15][cH:14][c:13](-[c:12]2[cH:11][cH:10][c:9]([C:7]([CH2:6][C:5]3([C:3]([O:2][CH3:1])=[O:4])[CH2:22][CH2:23][O:24][CH2:25][CH2:26]3)=[O:8])[cH:21][cH:20]2)[cH:19][cH:18]1>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([CH2:6][C:7](=[O:8])[c:9]2[cH:10][cH:11][c:12](-[c:13]3[cH:14][cH:15][c:16]([NH2:17])[cH:18...
COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCOCC1
COC(=O)C1(CC(=O)c2ccc(-c3ccc(N)cc3)cc2)CCOCC1
null
[Fe]
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C(CC1CCOCC1)c1ccc(-c2ccccc2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
91.4
[{"value": 91.0, "product": "NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.4, "product": "NC1=CC=C(C=C1)C1=CC=C(C=C1)C(CC1(CCOCC1)C(=O)OC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of methyl 4-[2-(4′-nitro-1,1′-biphenyl-4-yl)-2-oxoethyl]tetrahydro-2H-pyran-4-carboxylate (1.24 g, 3.25 mmol) in 85% ethanol (50 mL) was added iron powder (1.81 g), followed by 2 N aqueous HCl (1.62 mL), and the resulting mixture was refluxed for 2.5 h. The mixture was then filtered through a pad of Celit...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccccc1.C1CCOCC1
Other
[Fe].C(C)O
null
null
COC(=O)C1(CC(=O)c2ccc(-c3ccc([N+](=O)[O-])cc3)cc2)CCOCC1>[Fe].C(C)O>COC(=O)C1(CC(=O)c2ccc(-c3ccc(N)cc3)cc2)CCOCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0c802f49817f42d6be8e2648cf3fa03e
COC(C)(C)OC.O=C(c1ccc(Br)cc1)[C@H]1CCCC[C@H]1C(=O)O>>COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(Br)cc1
BrC1=CC=C(C(=O)[C@@H]2[C@@H](CCCC2)C(=O)O)C=C1.COC(C)(C)OC.Cl>>BrC1=CC=C(C(=O)[C@@H]2[C@@H](CCCC2)C(=O)OC)C=C1
COC(C)(C)O[CH3:1].[OH:2][C:3](=[O:4])[C@@H:5]1[CH2:6][CH2:7][CH2:8][CH2:9][C@@H:10]1[C:11](=[O:12])[c:13]1[cH:14][cH:15][c:16]([Br:17])[cH:18][cH:19]1>>[CH3:1][O:2][C:3](=[O:4])[C@@H:5]1[CH2:6][CH2:7][CH2:8][CH2:9][C@@H:10]1[C:11](=[O:12])[c:13]1[cH:14][cH:15][c:16]([Br:17])[cH:18][cH:19]1
COC(C)(C)OC.O=C(c1ccc(Br)cc1)[C@H]1CCCC[C@H]1C(=O)O
COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(Br)cc1
null
null
CO
Heteroatom Alkylation and Arylation
O-methylation
996ec4961b01515261a54c290b3ca2791e1cd44e68716f1a7d216a92013249dc
f1d0c21bce3f84df8e09e027f5fecc48c78a31aaf69561ba0dce25419b3c823e
O=C(c1ccccc1)C1CCCCC1
C-O-C(-C)(-C)-O-[CH3;D1;+0:1].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
42.1
[{"value": 42.0, "product": "BrC1=CC=C(C(=O)[C@@H]2[C@@H](CCCC2)C(=O)OC)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 42.1, "product": "BrC1=CC=C(C(=O)[C@@H]2[C@@H](CCCC2)C(=O)OC)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
40
CELSIUS
3
DAY
To a solution of cis-2-(4-bromobenzoyl)-1-cyclohexanecarboxylic acid (4.0 g, 12.85 mmol) in MeOH (50 mL) was added 2,2-dimethoxypropane (2.01 g, 19.28 mmol) and HCl (4.0 M in dioxane, 1.20 mL). The resulting solution was stirred at 40° C. for 3 days, and then evaporated to dryness. The resulting residue was purified by...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ether.Ether
Ester
null
null
C1CCCCC1.c1ccccc1
HO-
CO
40
72
COC(C)(C)OC.O=C(c1ccc(Br)cc1)[C@H]1CCCC[C@H]1C(=O)O>CO>COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(Br)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f28078c0604c469b887a017ec7139846
COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(Br)cc1.Nc1ccc(B(O)O)cc1>>COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(-c2ccc(N)cc2)cc1
C(=O)([O-])[O-].[Na+].[Na+].BrC1=CC=C(C(=O)[C@@H]2[C@@H](CCCC2)C(=O)OC)C=C1.NC1=CC=C(C=C1)B(O)O.ClCCl>>NC1=CC=C(C=C1)C1=CC=C(C=C1)C(=O)[C@@H]1[C@@H](CCCC1)C(=O)OC
Br[c:16]1[cH:15][cH:14][c:13]([C:11]([C@@H:10]2[C@H:5]([C:3]([O:2][CH3:1])=[O:4])[CH2:6][CH2:7][CH2:8][CH2:9]2)=[O:12])[cH:25][cH:24]1.OB(O)[c:17]1[cH:18][cH:19][c:20]([NH2:21])[cH:22][cH:23]1>>[CH3:1][O:2][C:3](=[O:4])[C@@H:5]1[CH2:6][CH2:7][CH2:8][CH2:9][C@@H:10]1[C:11](=[O:12])[c:13]1[cH:14][cH:15][c:16](-[c:17]2[cH...
COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(Br)cc1.Nc1ccc(B(O)O)cc1
COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(-c2ccc(N)cc2)cc1
null
C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2]
CCOC(=O)C.CCO.C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
d79a78c79f0c392f0911481acf5c300cc98205269acdb93c24fb610a61c4c868
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
O=C(c1ccc(-c2ccccc2)cc1)C1CCCCC1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O-B(-O)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10]):[c:4]:[c:5]
null
[]
85
CELSIUS
null
null
Methyl cis-2-(4-bromobenzoyl)cyclohexanecarboxylate (1.76 g, 5.41 mmol) and 4-amino phenyl boronic acid (1.13 g, 6.49 mmol) were added to a clean dry flask under argon. Toluene (50 mL), EtOH (20 mL), and 3 M aqueous Na2CO3 (14 mL, 43 mmol) were added, and resulting solution was degassed for 30 minutes by using a flow o...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
C1CCCCC1.c1ccccc1.c1ccccc1
HBr.B
C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].CCOC(=O)C.CCO.C1(=CC=CC=C1)C
85
null
COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(Br)cc1.Nc1ccc(B(O)O)cc1>C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].CCOC(=O)C.CCO.C1(=CC=CC=C1)C>COC(=O)[C@@H]1CCCC[C@@H]1C(=O)c1ccc(-c2ccc(N)cc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-91ac4de46f3e4b839aeb0ff63fe2cf3e
C[Si](C)(C)CCO.O=C(O)[C@@H]1CCCC[C@H]1C(=O)c1ccc(Br)cc1>>C[Si](C)(C)CCOC(=O)[C@@H]1CCCC[C@H]1C(=O)c1ccc(Br)cc1
BrC1=CC=C(C(=O)[C@H]2[C@@H](CCCC2)C(=O)O)C=C1.C[Si](CCO)(C)C.CCN=C=NCCCN(C)C.O>>BrC1=CC=C(C(=O)[C@H]2[C@@H](CCCC2)C(=O)OCC[Si](C)(C)C)C=C1
[CH3:1][Si:2]([CH3:3])([CH3:4])[CH2:5][CH2:6][OH:7].O[C:8](=[O:9])[C@@H:10]1[CH2:11][CH2:12][CH2:13][CH2:14][C@H:15]1[C:16](=[O:17])[c:18]1[cH:19][cH:20][c:21]([Br:22])[cH:23][cH:24]1>>[CH3:1][Si:2]([CH3:3])([CH3:4])[CH2:5][CH2:6][O:7][C:8](=[O:9])[C@@H:10]1[CH2:11][CH2:12][CH2:13][CH2:14][C@H:15]1[C:16](=[O:17])[c:18]...
C[Si](C)(C)CCO.O=C(O)[C@@H]1CCCC[C@H]1C(=O)c1ccc(Br)cc1
C[Si](C)(C)CCOC(=O)[C@@H]1CCCC[C@H]1C(=O)c1ccc(Br)cc1
null
null
C(Cl)Cl
Protection
Esterification of Carboxylic Acids
070670f68a20c1021da94fabee54def4688122fb721af5f52cd5a03630845d0e
0d8a72b7375d91aa7263e766e03a3cb7c4fa91e27abcd590409ff03b98eed690
O=C(c1ccccc1)C1CCCCC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5]-[C:6]=[O;D1;H0:7].[C:8]-[C:9]-[OH;D1;+0:10]>>[C:4]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[O;H0;D2;+0:10]-[C:9]-[C:8])-[C:5]-[C:6]=[O;D1;H0:7]
37
[{"value": 37.0, "product": "BrC1=CC=C(C(=O)[C@H]2[C@@H](CCCC2)C(=O)OCC[Si](C)(C)C)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 36.9, "product": "BrC1=CC=C(C(=O)[C@H]2[C@@H](CCCC2)C(=O)OCC[Si](C)(C)C)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
DAY
To a solution of trans-2-(4-bromobenzoyl)cyclohexanecarboxylic acid (5.0 g, 16.07 mmol) in DCM (80 mL) was added 2-(trimethylsilyl)ethanol (2.1 g, 17.68 mmol), N,N′-dimethylamino-pyridine (98 mg, 0.80 mmol), and EDCI (4.0 g, 20.89 mmol). The resulting reaction mixture was stirred at rt for 2 days. Water was added, and ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary alcohol
Ester
null
null
C1CCCCC1.c1ccccc1
HO-
C(Cl)Cl
null
48
C[Si](C)(C)CCO.O=C(O)[C@@H]1CCCC[C@H]1C(=O)c1ccc(Br)cc1>C(Cl)Cl>C[Si](C)(C)CCOC(=O)[C@@H]1CCCC[C@H]1C(=O)c1ccc(Br)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4f34df0009af4ec5b9397ec1a5edea37
Brc1ccccc1.O=C1OC(=O)C2CC12>>O=C(c1ccc(Br)cc1)[C@H]1C[C@H]1C(=O)O
BrC1=CC=CC=C1.[Al+3].[Cl-].[Cl-].[Cl-].Cl.C12C(OC(C2C1)=O)=O>>BrC1=CC=C(C(=O)[C@@H]2[C@@H](C2)C(=O)O)C=C1
[cH:3]1[cH:4][cH:5][c:6]([Br:7])[cH:8][cH:9]1.[O:1]=[C:2]1[CH:10]2[CH2:11][CH:12]2[C:13](=[O:14])[O:15]1>>[O:1]=[C:2]([c:3]1[cH:4][cH:5][c:6]([Br:7])[cH:8][cH:9]1)[C@H:10]1[CH2:11][C@H:12]1[C:13](=[O:14])[OH:15]
Brc1ccccc1.O=C1OC(=O)C2CC12
O=C(c1ccc(Br)cc1)[C@H]1C[C@H]1C(=O)O
null
null
C(Cl)Cl
C-C Coupling
OtherReaction
36efb843272085513718adf2456d27080e06914a2cf60547cbc37c7344b11e9f
4836357c99dfeeac9d5083fedc379181a858ae45ac77bd85eb46e7e1a9df36f0
O=C(c1ccccc1)C1CC1
[O;D1;H0:1]=[C:2]1-[O;H0;D2;+0:3]-[C;H0;D3;+0:4](=[O;D1;H0:5])-[CH;D3;+0:6]2-[C:7]-[CH;D3;+0:8]-1-2.[c:9]:[c:10]:[cH;D2;+0:11]:[c:12]:[c:13]>>[O;D1;H0:1]=[C:2](-[OH;D1;+0:3])-[C@@H;D3;+0:8]1-[C:7]-[C@@H;D3;+0:6]-1-[C;H0;D3;+0:4](=[O;D1;H0:5])-[c;H0;D3;+0:11](:[c:10]:[c:9]):[c:12]:[c:13]
74.6
[{"value": 65.0, "product": "BrC1=CC=C(C(=O)[C@@H]2[C@@H](C2)C(=O)O)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 74.6, "product": "BrC1=CC=C(C(=O)[C@@H]2[C@@H](C2)C(=O)O)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
DAY
To a cold (0° C.) stirred solution of bromobenzene (9.09 g, 57.89 mmol) and AlCl3 (18.36 g, 137.84 mmol) in dry DCM (150 mL) was added 3-oxabicyclo[3.1.0]hexane-2,4-dione (5.40 g, 48.24 mmol). The reaction mixture was stirred at rt for 3 days. The dark-red solution was then poured into ice-cold water (120 mL), and conc...
10.6084/m9.figshare.5104873.v1
null
Anhydride
Carboxylic acid.Ketone
c1ccccc1.C1OCC2CC12
c1ccccc1
c1ccccc1.C1CC1
null
C(Cl)Cl
null
72
Brc1ccccc1.O=C1OC(=O)C2CC12>C(Cl)Cl>O=C(c1ccc(Br)cc1)[C@H]1C[C@H]1C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2fd5618e389a417881c57b535e63dc15
COC(C)(C)OC.O=C(c1ccc(Br)cc1)[C@H]1C[C@H]1C(=O)O>>COC(=O)[C@@H]1C[C@@H]1C(=O)c1ccc(Br)cc1
BrC1=CC=C(C(=O)[C@@H]2[C@@H](C2)C(=O)O)C=C1.COC(C)(C)OC.Cl>>BrC1=CC=C(C(=O)[C@@H]2[C@@H](C2)C(=O)OC)C=C1
COC(C)(C)O[CH3:1].[OH:2][C:3](=[O:4])[C@@H:5]1[CH2:6][C@@H:7]1[C:8](=[O:9])[c:10]1[cH:11][cH:12][c:13]([Br:14])[cH:15][cH:16]1>>[CH3:1][O:2][C:3](=[O:4])[C@@H:5]1[CH2:6][C@@H:7]1[C:8](=[O:9])[c:10]1[cH:11][cH:12][c:13]([Br:14])[cH:15][cH:16]1
COC(C)(C)OC.O=C(c1ccc(Br)cc1)[C@H]1C[C@H]1C(=O)O
COC(=O)[C@@H]1C[C@@H]1C(=O)c1ccc(Br)cc1
null
null
CO
Heteroatom Alkylation and Arylation
O-methylation
996ec4961b01515261a54c290b3ca2791e1cd44e68716f1a7d216a92013249dc
f1d0c21bce3f84df8e09e027f5fecc48c78a31aaf69561ba0dce25419b3c823e
O=C(c1ccccc1)C1CC1
C-O-C(-C)(-C)-O-[CH3;D1;+0:1].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
99.7
[{"value": 99.0, "product": "BrC1=CC=C(C(=O)[C@@H]2[C@@H](C2)C(=O)OC)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.7, "product": "BrC1=CC=C(C(=O)[C@@H]2[C@@H](C2)C(=O)OC)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
40
CELSIUS
3
DAY
To a solution of cis-2-(4-bromobenzoyl)cyclopropanecarboxylic acid (10.6 g, 36.63 mmol) in MeOH (250 mL) was added 2,2-dimethoxypropane (9.54 g, 91.59 mmol) and HCl (4.0 M in dioxane, 3.50 mL). The resulting solution was stirred at 40° C. for 3 days, and then evaporated to dryness. The resulting residue was purified by...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ether.Ether
Ester
null
null
C1CC1.c1ccccc1
HO-
CO
40
72
COC(C)(C)OC.O=C(c1ccc(Br)cc1)[C@H]1C[C@H]1C(=O)O>CO>COC(=O)[C@@H]1C[C@@H]1C(=O)c1ccc(Br)cc1