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-58ac291c943e4c7ab3a44a9faf264ba6
CCN.CO[C@@H]1O[C@H](C(=O)O)[C@@H]2OC(C)(C)O[C@@H]12>>CCNC(=O)[C@H]1O[C@@H](OC)[C@@H]2OC(C)(C)O[C@@H]21
C(C)OCC.C(C(=O)Cl)(=O)Cl.CO[C@@H]1O[C@@H]([C@H]2[C@H]1OC(O2)(C)C)C(=O)O.C(C)N>>C(C)NC(=O)[C@H]1O[C@H]([C@@H]2OC(O[C@@H]21)(C)C)OC
[CH3:1][CH2:2][NH2:3].O[C:4](=[O:5])[C@H:6]1[O:7][C@@H:8]([O:9][CH3:10])[C@@H:11]2[O:12][C:13]([CH3:14])([CH3:15])[O:16][C@@H:17]12>>[CH3:1][CH2:2][NH:3][C:4](=[O:5])[C@H:6]1[O:7][C@@H:8]([O:9][CH3:10])[C@@H:11]2[O:12][C:13]([CH3:14])([CH3:15])[O:16][C@H:17]12
CCN.CO[C@@H]1O[C@H](C(=O)O)[C@@H]2OC(C)(C)O[C@@H]12
CCNC(=O)[C@H]1O[C@@H](OC)[C@@H]2OC(C)(C)O[C@@H]21
null
CN(C=O)C.CN(C=O)C
ClCCl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
C1O[C@H]2COC[C@H]2O1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[#8:4]-[C:5])-[C:6]-[#8:7].[C;D1;H3:8]-[C:9]-[NH2;D1;+0:10]>>[#8:7]-[C:6]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:10]-[C:9]-[C;D1;H3:8])-[#8:4]-[C:5]
94.1
[{"value": 94.1, "product": "C(C)NC(=O)[C@H]1O[C@H]([C@@H]2OC(O[C@@H]21)(C)C)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
Oxalyl chloride (14.0 ml, 160 mmol) was added dropwise to a stirred solution of (3aR,4S,6R,6aR)-6-methoxy-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxole-4-carboxylic acid (J. Amer. Chem. Soc., 80, 5168–5173 (1958)) (23.30 g, 107 mmol) in anhydrous dichloromethane (120 ml) and N,N-dimethylformamide (2 drops) and the mixt...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
C1O[C@H]2COC[C@H]2O1
HO-
CN(C=O)C.CN(C=O)C.ClCCl
null
3
CCN.CO[C@@H]1O[C@H](C(=O)O)[C@@H]2OC(C)(C)O[C@@H]12>CN(C=O)C.CN(C=O)C.ClCCl>CCNC(=O)[C@H]1O[C@@H](OC)[C@@H]2OC(C)(C)O[C@@H]21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4a65621b973a4cf9ad3c7036ebba211a
CC(=O)OC[C@H]1O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]1OC(C)=O.COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1>>COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1
C/C(=N\[Si](C)(C)C)/O[Si](C)(C)C.C1(=CC=CC=C1)C(CNC1=C2N=CNC2=NC(=N1)C(=O)OC)C1=CC=CC=C1.C(C)(=O)O[C@H]1[C@H](OC(C)=O)[C@H](OC(C)=O)[C@H](O1)COC(C)=O.FC(S(=O)(=O)O[Si](C)(C)C)(F)F>>C(C)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C)=O)COC(C)=O)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OC
CC(=O)O[C@@H:27]1[O:28][C@H:29]([CH2:30][O:31][C:32]([CH3:33])=[O:34])[C@@H:35]([O:36][C:37]([CH3:38])=[O:39])[C@H:40]1[O:41][C:42]([CH3:43])=[O:44].[CH3:1][O:2][C:3](=[O:4])[c:5]1[n:6][c:7]([NH:8][CH2:9][CH:10]([c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[c:23]2[n:24][cH:25]...
CC(=O)OC[C@H]1O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]1OC(C)=O.COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1
null
null
ClC(C)(Cl)Cl.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
a90222e67a4a22678b87b59d1ecec052c8245214c445cc6a40c830f6056425a0
555d70919b361b350c80f46e885ff5cda87616c212c907f1056db36bb1eb2375
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
C-C(=O)-O-[C@@H;D3;+0:1]1-[#8:2]-[C:3]-[C:4]-[C:5]-1-[#8:6]-[C:7](-[C;D1;H3:8])=[O;D1;H0:9].[#8:10]-[C:11](=[O;D1;H0:12])-[c:13]1:[#7;a:14]:[c:15]2:[nH;D2;+0:16]:[c:17]:[#7;a:18]:[c:19]:2:[c:20]:[#7;a:21]:1>>[#8:10]-[C:11](=[O;D1;H0:12])-[c:13]1:[#7;a:14]:[c:15]2:[c:19](:[#7;a:18]:[c:17]:[n;H0;D3;+0:16]:2-[C@@H;D3;+0:1...
80.7
[{"value": 80.7, "product": "C(C)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C)=O)COC(C)=O)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A suspension of methyl 6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 7) (1.5 g, 4.02 mmol) in 1,1,1-trichloroethane (40 ml) was treated with N,O-bis(trimethylsilyl)acetamide (4.8 ml, 19.6 mmol). The mixture was heated under reflux for two hours. The solution was allowed to cool to room temperature a...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether
Ether
C1CCOC1.c1ncc2[nH]cnc2n1
c1ncc2[nH]cnc2n1.C1CCOC1
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOC1
HO-
ClC(C)(Cl)Cl.C(C)(=O)OCC
null
null
CC(=O)OC[C@H]1O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]1OC(C)=O.COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1>ClC(C)(Cl)Cl.C(C)(=O)OCC>COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3bfef3acea604c6e95d59fcc73d37c77
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1>>COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
C(C)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C)=O)COC(C)=O)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OC.C([O-])([O-])=O.[Na+].[Na+]>>O[C@H]1[C@@H](O[C@@H]([C@H]1O)CO)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OC
CC(=O)[O:31][CH2:30][C@H:29]1[O:28][C@@H:27]([n:26]2[cH:25][n:24][c:23]3[c:7]([NH:8][CH2:9][CH:10]([c:11]4[cH:12][cH:13][cH:14][cH:15][cH:16]4)[c:17]4[cH:18][cH:19][cH:20][cH:21][cH:22]4)[n:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[n:37][c:36]32)[C@H:34]([O:35]C(C)=O)[C@@H:32]1[O:33]C(C)=O>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[n:6...
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
null
null
CO
Reduction
OtherReaction
b1205f31a625dd524c4abcf6ea407c1a38966308677d8535d59411f69b7afe49
53784a05a6c1858c11deb702d4a1392e7852c783da9a57d4771755f87682c932
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
C-C(=O)-[O;H0;D2;+0:1]-[C:2]-[C:3]1-[#8:4]-[C:5]-[C:6](-[O;H0;D2;+0:7]-C(-C)=O)-[C:8]-1-[O;H0;D2;+0:9]-C(-C)=O>>[OH;D1;+0:1]-[C:2]-[C:3]1-[#8:4]-[C:5]-[C:6](-[OH;D1;+0:7])-[C:8]-1-[OH;D1;+0:9]
93.6
[{"value": 93.6, "product": "O[C@H]1[C@@H](O[C@@H]([C@H]1O)CO)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of methyl 9-{(2R,3R,4R,5R)-3,4-bis(acetyloxy)-5-[(acetyloxy)methyl]-tetrahydro-2-furanyl}-6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 15) (2.0 g, 3.17 mmol), sodium carbonate (35 mg) and dry methanol (40 ml) was stirred at room temperature for 3.5 hours. The solvent was removed under re...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Ester
Primary alcohol.Secondary alcohol.Secondary alcohol
null
null
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOC1
HO-
CO
null
null
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1>CO>COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-32838b2a0dea4bfebe8540de2786d989
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1.NCCN>>NCCNC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
O[C@H]1[C@@H](O[C@@H]([C@H]1O)CO)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OC.C(CN)N>>NCCNC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)CO)NCC(C1=CC=CC=C1)C1=CC=CC=C1
CO[C:5](=[O:6])[c:7]1[n:8][c:9]([NH:10][CH2:11][CH:12]([c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[c:19]2[cH:20][cH:21][cH:22][cH:23][cH:24]2)[c:25]2[n:26][cH:27][n:28]([C@@H:29]3[O:30][C@H:31]([CH2:32][OH:33])[C@@H:34]([OH:35])[C@H:36]3[OH:37])[c:38]2[n:39]1.[NH2:1][CH2:2][CH2:3][NH2:4]>>[NH2:1][CH2:2][CH2:3][NH:4][C...
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1.NCCN
NCCNC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
null
null
ClCCl
Acylation
Aminolysis of esters
04c54ce22aa9bc0cea0de3d900446bcab51cf02bebeb606fa788a47dcd0e37ff
4335147c9ad02004b7c12428d7eac0b2e7e0e2017adc471d01c387239de8017d
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[#7;a:4]:[c:5](:[#7;a:6]):[c:7](:[#7;a:8]):[c:9]:[#7;a:10]:1.[C:11]-[C:12]-[NH2;D1;+0:13]>>[#7;a:8]:[c:7]1:[c:9]:[#7;a:10]:[c:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:13]-[C:12]-[C:11]):[#7;a:4]:[c:5]:1:[#7;a:6]
78.2
[{"value": 78.0, "product": "NCCNC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)CO)NCC(C1=CC=CC=C1)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.2, "product": "NCCNC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)CO)NCC(C1=CC=CC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCEN...
105
CELSIUS
null
null
A mixture of methyl 9-[(2R,3R,4S,5R)-3,4-dihydroxy-5-(hydroxymethyl)tetrahydro-2-furanyl]-6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 16) (0.52 g, 1.03 mmol) and 1,2-ethylenediamine (0.6 g, 10 mmol) was heated at 105° C. for 3 hours. The mixture was dissolved in a little dichloromethane and purifi...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOC1
HO-
ClCCl
105
null
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1.NCCN>ClCCl>NCCNC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7efd89374aa24ed08aa7d37e2d91e9b1
CC(C)C1CCNCC1.O=C1c2ccccc2C(=O)N1CCBr>>CC(C)C1CCN(CCN2C(=O)c3ccccc3C2=O)CC1
C(C)(C)C1CCNCC1.BrCCN1C(C=2C(C1=O)=CC=CC2)=O.C([O-])([O-])=O.[K+].[K+]>>C(C)(C)C1CCN(CC1)CCN1C(C2=CC=CC=C2C1=O)=O
[CH3:1][CH:2]([CH3:3])[CH:4]1[CH2:5][CH2:6][NH:7][CH2:21][CH2:22]1.Br[CH2:8][CH2:9][N:10]1[C:11](=[O:12])[c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]2[C:19]1=[O:20]>>[CH3:1][CH:2]([CH3:3])[CH:4]1[CH2:5][CH2:6][N:7]([CH2:8][CH2:9][N:10]2[C:11](=[O:12])[c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]3[C:19]2=[O:20])[CH2:21][CH2:22...
CC(C)C1CCNCC1.O=C1c2ccccc2C(=O)N1CCBr
CC(C)C1CCN(CCN2C(=O)c3ccccc3C2=O)CC1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
0240b8450ff2c489d02f5f0d90bc953079d7a3ab239d35a03f26392fc248b4ef
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
O=C1c2ccccc2C(=O)N1CCN1CCCCC1
Br-[CH2;D2;+0:1]-[C:2]-[#7:3](-[C:4]=[O;D1;H0:5])-[C:6]=[O;D1;H0:7].[C:8]-[C:9]-[NH;D2;+0:10]-[C:11]-[C:12]>>[C:8]-[C:9]-[N;H0;D3;+0:10](-[CH2;D2;+0:1]-[C:2]-[#7:3](-[C:4]=[O;D1;H0:5])-[C:6]=[O;D1;H0:7])-[C:11]-[C:12]
54.4
[{"value": 54.4, "product": "C(C)(C)C1CCN(CC1)CCN1C(C2=CC=CC=C2C1=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of 4-isopropylpiperidine (3.3 g, 20.2 mmol), N-(2-bromoethyl)phthalimide (5.4 g, 21.3 mmol), potassium carbonate (5.9 g, 45.4 mmol) and acetonitrile (100 ml) and was heated under reflux for 2.5 hours then stirred at room temperature overnight. The solvent was removed under reduced pressure and the residue pa...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccc2c(c1)C[NH]C2
HBr
C(C)#N
null
8
CC(C)C1CCNCC1.O=C1c2ccccc2C(=O)N1CCBr>C(C)#N>CC(C)C1CCN(CCN2C(=O)c3ccccc3C2=O)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a37b355baf0d4ccb87189a29d7e7e818
CC(C)=O.NC1CCCC1>>CC(C)NC1CCCC1
C1(CCCC1)N.CC(=O)C>>C(C)(C)NC1CCCC1
O=[C:2]([CH3:1])[CH3:3].[NH2:4][CH:5]1[CH2:6][CH2:7][CH2:8][CH2:9]1>>[CH3:1][CH:2]([CH3:3])[NH:4][CH:5]1[CH2:6][CH2:7][CH2:8][CH2:9]1
CC(C)=O.NC1CCCC1
CC(C)NC1CCCC1
null
[OH-].[OH-].[Pd+2]
null
Heteroatom Alkylation and Arylation
Reductive amination with ketone
4940e8ed9a0db9bde699fdcdc3aff2cff0409c19478aa0ed1acfd98213338adf
07faf85ffe990e88a1de7fd04a339bf226f78d8bfae9712ea59eebd76bb54b9f
C1CCCC1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[C;D1;H3:3].[C:4]-[C:5](-[NH2;D1;+0:6])-[C:7]>>[C:4]-[C:5](-[NH;D2;+0:6]-[CH;D3;+0:1](-[C;D1;H3:2])-[C;D1;H3:3])-[C:7]
null
[]
null
null
null
null
Peariman's catalyst (20% w/w palladium hydroxide-on-carbon) (1.5 g) was added to a solution of cyclopentylamine (15 ml, 0.21 mol) in acetone (200 ml). The reaction mixture was stirred under an atmosphere of hydrogen gas at 414 kPa (60 psi). After stirring for 16 hours the reaction mixture was filtered through Arbocel (...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
Secondary amine
null
null
C1CCCC1
Other
[OH-].[OH-].[Pd+2]
null
null
CC(C)=O.NC1CCCC1>[OH-].[OH-].[Pd+2]>CC(C)NC1CCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2edc0f68f55d4d2e9a504b31994f60af
CC(C)NC1CCCC1.N#CCO>>CC(C)N(CC#N)C1CCCC1
OCC#N.C(C)(C)NC1CCCC1>>C1(CCCC1)N(C(C)C)CC#N
[CH3:1][CH:2]([CH3:3])[NH:4][CH:8]1[CH2:9][CH2:10][CH2:11][CH2:12]1.O[CH2:5][C:6]#[N:7]>>[CH3:1][CH:2]([CH3:3])[N:4]([CH2:5][C:6]#[N:7])[CH:8]1[CH2:9][CH2:10][CH2:11][CH2:12]1
CC(C)NC1CCCC1.N#CCO
CC(C)N(CC#N)C1CCCC1
null
null
O.C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
f33a8d71b7dbaa463dcb87d1e5073e084c21a5fbc935ce82a22b6d65293f45d1
87693a475e46c41583976158ec46dcaf8be8cc05c5635654a6a68033770f8d5c
C1CCCC1
O-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3].[C:4]-[C:5](-[NH;D2;+0:6]-[C:7](-[C;D1;H3:8])-[C;D1;H3:9])-[C:10]>>[C:4]-[C:5](-[N;H0;D3;+0:6](-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3])-[C:7](-[C;D1;H3:8])-[C;D1;H3:9])-[C:10]
null
[]
null
null
null
null
Hydroxyacetonitrile (8.2 ml of a 70% w/w solution in water, 0.1 mol) was added to a solution of N-isopropylcyclopentanamine (11.43 g, 0.09 mol) (Preparation 23) in ethanol (60 ml). The reaction mixture was heated under reflux for 3 hours, allowed to cool and the solvent removed under reduced pressure. The residue was p...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Secondary amine
Tertiary amine
null
null
C1CCCC1
HO-
O.C(C)O
null
null
CC(C)NC1CCCC1.N#CCO>O.C(C)O>CC(C)N(CC#N)C1CCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6a39682c48824103b1827335e43915c2
CC(C)N(CC#N)C1CCCC1>>CC(C)N(CCN)C1CCCC1
[OH-].[Na+].[H-].[Al+3].[Li+].[H-].[H-].[H-].C1(CCCC1)N(C(C)C)CC#N.O>>C1(CCCC1)N(CCN)C(C)C
[CH3:1][CH:2]([CH3:3])[N:4]([CH2:5][C:6]#[N:7])[CH:8]1[CH2:9][CH2:10][CH2:11][CH2:12]1>>[CH3:1][CH:2]([CH3:3])[N:4]([CH2:5][CH2:6][NH2:7])[CH:8]1[CH2:9][CH2:10][CH2:11][CH2:12]1
CC(C)N(CC#N)C1CCCC1
CC(C)N(CCN)C1CCCC1
null
null
O1CCCC1
Reduction
Reduction of nitrile to amine
65bec2d9f430701d30dc9fcbe1c5418f3dfa174d67be035c50edfc71895dc9c7
e8d1bc928b94bd4f5bf4b23363ce8f88b1ce7d146ba93829e7b8ad8dbe0007a7
C1CCCC1
[#7:1]-[C:2]-[C;H0;D2;+0:3]#[N;H0;D1;+0:4]>>[#7:1]-[C:2]-[CH2;D2;+0:3]-[NH2;D1;+0:4]
9.2
[{"value": 9.2, "product": "C1(CCCC1)N(CCN)C(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
20
MINUTE
Lithium aluminium hydride (66 ml of a 1 molar solution in tetrahydrofuran, 0.066 mol) was added to a stirred solution of [cyclopentyl(isopropyl)amino]acetonitrile (10 g, 0.66 mol) (Preparation 24) in tetrahydrofuran (100 ml) at 0° C. The reaction mixture was stirred at 0° C. for 20 minutes and then heated under reflux ...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
C1CCCC1
null
O1CCCC1
0
0.333333
CC(C)N(CC#N)C1CCCC1>O1CCCC1>CC(C)N(CCN)C1CCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2b195feacae64a78b2bbb43fd351fd03
CC(C)NC1CCCCC1.N#CCO>>CC(C)N(CC#N)C1CCCCC1
C(C)(C)NC1CCCCC1.OCC#N>>C1(CCCCC1)N(C(C)C)CC#N
[CH3:1][CH:2]([CH3:3])[NH:4][CH:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1.O[CH2:5][C:6]#[N:7]>>[CH3:1][CH:2]([CH3:3])[N:4]([CH2:5][C:6]#[N:7])[CH:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1
CC(C)NC1CCCCC1.N#CCO
CC(C)N(CC#N)C1CCCCC1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
f33a8d71b7dbaa463dcb87d1e5073e084c21a5fbc935ce82a22b6d65293f45d1
87693a475e46c41583976158ec46dcaf8be8cc05c5635654a6a68033770f8d5c
C1CCCCC1
O-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3].[C:4]-[C:5](-[NH;D2;+0:6]-[C:7](-[C;D1;H3:8])-[C;D1;H3:9])-[C:10]>>[C:4]-[C:5](-[N;H0;D3;+0:6](-[CH2;D2;+0:1]-[C:2]#[N;D1;H0:3])-[C:7](-[C;D1;H3:8])-[C;D1;H3:9])-[C:10]
null
[]
null
null
null
null
Prepared from N-isopropylcyclohexylamine and hydroxyacetonitrile by a similar method to Preparation 24. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Secondary amine
Tertiary amine
null
null
C1CCCCC1
HO-
null
null
null
CC(C)NC1CCCCC1.N#CCO>>CC(C)N(CC#N)C1CCCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f2ee14fab341482e9a74a7bb84f63a09
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NCCCN>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCCN)nc32)[C@H](O)[C@@H]1O
C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)OC)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1.NCCCN>>NCCCNC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)NCC(C1=CC=CC=C1)C1=CC=CC=C1
CO[C:31]([c:30]1[n:29][c:13]([NH:14][CH2:15][CH:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[c:12]2[n:11][cH:10][n:9]([C@@H:8]3[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:42]([OH:43])[C@H:40]3[OH:41])[c:39]2[n:38]1)=[O:32].[NH2:33][CH2:34][CH2:35][CH2:36][NH2:37]...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NCCCN
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCCN)nc32)[C@H](O)[C@@H]1O
null
null
ClCCl
Acylation
Aminolysis of esters
04c54ce22aa9bc0cea0de3d900446bcab51cf02bebeb606fa788a47dcd0e37ff
4335147c9ad02004b7c12428d7eac0b2e7e0e2017adc471d01c387239de8017d
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[#7;a:10]:1.[C:11]-[C:12]-[NH2;D1;+0:13]>>[#7;a:7]:[c:6]1:[c:5]:[#7;a:4]:[c:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:13]-[C:12]-[C:11]):[#7;a:10]:[c:8]:1:[#7;a:9]
58.4
[{"value": 58.0, "product": "NCCCNC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)NCC(C1=CC=CC=C1)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 58.4, "product": "NCCCNC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)NCC(C1=CC=CC=C1)C1=CC=CC=C1", "details": "CA...
100
CELSIUS
null
null
A mixture of methyl 6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxylate (Preparation 9) (0.35 g, 0.64 mmol) and 1,3-diaminopropane (0.45 g, 6.1 mmol) was heated at 100° C. for 3 hours. The mixture was dissolved in a little dichloromethane and...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Secondary amide
null
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1
HO-
ClCCl
100
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NCCCN>ClCCl>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCCN)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9a7c7421a5744e4b9cb52f422cdeec91
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NC1CCN(Cc2ccccc2)CC1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCN(Cc5ccccc5)CC4)nc32)[C@H](O)[C@@H]1O
C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)OC)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1.C(C1=CC=CC=C1)N1CCC(CC1)N>>C(C1=CC=CC=C1)N1CCC(CC1)NC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)NCC(C1=CC=CC=C1)C1=CC=CC=C1
CO[C:31]([c:30]1[n:29][c:13]([NH:14][CH2:15][CH:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[c:12]2[n:11][cH:10][n:9]([C@@H:8]3[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:51]([OH:52])[C@H:49]3[OH:50])[c:48]2[n:47]1)=[O:32].[NH2:33][CH:34]1[CH2:35][CH2:36][N:37]([...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NC1CCN(Cc2ccccc2)CC1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCN(Cc5ccccc5)CC4)nc32)[C@H](O)[C@@H]1O
null
null
ClCCl
Acylation
Aminolysis of esters
04c54ce22aa9bc0cea0de3d900446bcab51cf02bebeb606fa788a47dcd0e37ff
4335147c9ad02004b7c12428d7eac0b2e7e0e2017adc471d01c387239de8017d
O=C(NC1CCN(Cc2ccccc2)CC1)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@H]3CCCO3)c2n1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[#7;a:10]:1.[C:11]-[C:12](-[NH2;D1;+0:13])-[C:14]>>[#7;a:7]:[c:6]1:[c:5]:[#7;a:4]:[c:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:13]-[C:12](-[C:11])-[C:14]):[#7;a:10]:[c:8]:1:[#7;a:9]
80
[{"value": 80.0, "product": "C(C1=CC=CC=C1)N1CCC(CC1)NC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)NCC(C1=CC=CC=C1)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.5, "product": "C(C1=CC=CC=C1)N1CCC(CC1)NC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)NCC(...
105
CELSIUS
null
null
A mixture of methyl 6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxylate (Preparation 9) (1.0 g, 1.83 mmol) and 1-benzyl-4-piperidinylamine (2.4 ml, 11 mmol) was heated at 105° C. for 4 hours. The mixture was dissolved in a little dichlorometh...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Secondary amide
null
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CC[NH]CC1.c1ccccc1
HO-
ClCCl
105
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NC1CCN(Cc2ccccc2)CC1>ClCCl>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCN(Cc5ccccc5)CC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9f53c36c189340a68a9f5c76b3e8b421
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCN(Cc5ccccc5)CC4)nc32)[C@H](O)[C@@H]1O>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCNCC4)nc32)[C@H](O)[C@@H]1O
C(C1=CC=CC=C1)N1CCC(CC1)NC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)NCC(C1=CC=CC=C1)C1=CC=CC=C1.C(=O)[O-].[NH4+]>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NC1CCNCC1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1
c1ccc(C[N:37]2[CH2:36][CH2:35][CH:34]([NH:33][C:31]([c:30]3[n:29][c:13]([NH:14][CH2:15][CH:16]([c:17]4[cH:18][cH:19][cH:20][cH:21][cH:22]4)[c:23]4[cH:24][cH:25][cH:26][cH:27][cH:28]4)[c:12]4[n:11][cH:10][n:9]([C@@H:8]5[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:44]([OH:45])[C@H:42]5[OH:43])[c:41]4[n:40]3)=[O:3...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCN(Cc5ccccc5)CC4)nc32)[C@H](O)[C@@H]1O
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCNCC4)nc32)[C@H](O)[C@@H]1O
null
[OH-].[Pd+2].[OH-]
C(C)O
Deprotection
Hydrogenolysis of tertiary amines
cd3c1aa319cad45f383f17cc0b8bfc8337d7078d779f654933f9a447e64292a5
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
O=C(NC1CCNCC1)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@H]3CCCO3)c2n1
[C:1]-[C:2]-[N;H0;D3;+0:3](-C-c1:c:c:c:c:c:1)-[C:4]-[C:5]>>[C:1]-[C:2]-[NH;D2;+0:3]-[C:4]-[C:5]
null
[]
null
null
null
null
A solution of N-(1-benzyl-4-piperidinyl)-6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxamide (Preparation 33) (1.03 g, 1.47 mmol), palladium (II) hydroxide (0.9 g) and ammonium formate (0.46 g, 7.3 mmol) in ethanol (10 ml) was heated under re...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.C1CC[NH]CC1
C1CCNCC1
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CCNCC1
Other
[OH-].[Pd+2].[OH-].C(C)O
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCN(Cc5ccccc5)CC4)nc32)[C@H](O)[C@@H]1O>[OH-].[Pd+2].[OH-].C(C)O>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NC4CCNCC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-642fdc49fd4040db955ddee96ee5402b
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@H](O)[C@@H]1O
C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)OC)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1.[OH-].[Na+].Cl>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)O)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1
C[O:33][C:31]([c:30]1[n:29][c:13]([NH:14][CH2:15][CH:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[c:12]2[n:11][cH:10][n:9]([C@@H:8]3[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:38]([OH:39])[C@H:36]3[OH:37])[c:35]2[n:34]1)=[O:32]>>[CH3:1][CH2:2][NH:3][C:4](=[O:5])[...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@H](O)[C@@H]1O
null
null
CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4](:[#7;a:5]):[#7;a:6]>>[#7;a:5]:[c:4](-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]):[#7;a:6]
30.8
[{"value": 30.0, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)O)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 30.8, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)O)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1", "details": "CALCUL...
null
null
null
null
A solution of methyl 6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxylate (Preparation 9) (0.7 g, 1.28 mmol) and 10% w/w aqueous sodium hydroxide solution (1.3 ml, 3.2 mmol) in methanol (2.3 ml) was stirred at room temperature for 14 hours. Th...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1
Other
CO
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O>CO>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-061f27f5257242b2996f0872243ec48d
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@H](O)[C@@H]1O.O=C(NC1CCNCC1)C(F)(F)F>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(NC(=O)C(F)(F)F)CC4)nc32)[C@H](O)[C@@H]1O
C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)O)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1.FC(C(=O)NC1CCNCC1)(F)F.Cl.CN(CCCN=C=NCC)C>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)N1CCC(CC1)NC(C(F)(F)F)=O)[C@H]1[C@@H]([C@@H]([C@H](O1)C(=O)NCC)O)O)C1=CC=CC=C1
O[C:31]([c:30]1[n:29][c:13]([NH:14][CH2:15][CH:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[c:12]2[n:11][cH:10][n:9]([C@@H:8]3[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:50]([OH:51])[C@H:48]3[OH:49])[c:47]2[n:46]1)=[O:32].[NH:33]1[CH2:34][CH2:35][CH:36]([NH:37][C...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@H](O)[C@@H]1O.O=C(NC1CCNCC1)C(F)(F)F
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(NC(=O)C(F)(F)F)CC4)nc32)[C@H](O)[C@@H]1O
null
null
ClCCl
Acylation
Acylation of Nitrogen Nucleophiles by Carboxylic Acids
fbfce93ec1ece674255bb96c5cec09ad611382b41cf117dfe580015e21744a71
c5e4172490b2731ba9322b68af56376edadc31ce0bb9a3dfdea23a1817a852fd
O=C(c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@H]3CCCO3)c2n1)N1CCCCC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3]1:[#7;a:4]:[c:5]:[c:6](:[#7;a:7]):[c:8](:[#7;a:9]):[#7;a:10]:1.[C:11]-[C:12]-[NH;D2;+0:13]-[C:14]-[C:15]>>[#7;a:7]:[c:6]1:[c:5]:[#7;a:4]:[c:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:13](-[C:12]-[C:11])-[C:14]-[C:15]):[#7;a:10]:[c:8]:1:[#7;a:9]
null
[]
null
null
null
null
A solution of 6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxylic acid (Preparation 39) (0.2 g, 0.38 mmol), 2,2,2-trifluoro-N-(4-piperidinyl)acetamide (83 mg, 0.42 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (81 mg, 0...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Tertiary amide
C1CCNCC1
C1CC[NH]CC1
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CC[NH]CC1
HO-
ClCCl
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@H](O)[C@@H]1O.O=C(NC1CCNCC1)C(F)(F)F>ClCCl>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(NC(=O)C(F)(F)F)CC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dc41c535004c441f83b6625c12376dbc
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(NC(=O)C(F)(F)F)CC4)nc32)[C@H](O)[C@@H]1O>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(N)CC4)nc32)[C@H](O)[C@@H]1O
C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)N1CCC(CC1)NC(C(F)(F)F)=O)[C@H]1[C@@H]([C@@H]([C@H](O1)C(=O)NCC)O)O)C1=CC=CC=C1>>NC1CCN(CC1)C(=O)C1=NC(=C2N=CN(C2=N1)[C@H]1[C@@H]([C@@H]([C@H](O1)C(=O)NCC)O)O)NCC(C1=CC=CC=C1)C1=CC=CC=C1
O=C(C(F)(F)F)[NH:37][CH:36]1[CH2:35][CH2:34][N:33]([C:31]([c:30]2[n:29][c:13]([NH:14][CH2:15][CH:16]([c:17]3[cH:18][cH:19][cH:20][cH:21][cH:22]3)[c:23]3[cH:24][cH:25][cH:26][cH:27][cH:28]3)[c:12]3[n:11][cH:10][n:9]([C@@H:8]4[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:44]([OH:45])[C@H:42]4[OH:43])[c:41]3[n:40]2...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(NC(=O)C(F)(F)F)CC4)nc32)[C@H](O)[C@@H]1O
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(N)CC4)nc32)[C@H](O)[C@@H]1O
null
null
CO.N
Reduction
Hydrogenolysis of amides/imides/carbamates
44b36597c7daf0608965c52c8db8a9220c21d9447ce54e0af375898475f3493f
caaeb83af2cb178156ae90fe7f610a106cd4bb5397d23f56d37a7fe11e2668ed
O=C(c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@H]3CCCO3)c2n1)N1CCCCC1
F-C(-F)(-F)-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
101.7
[{"value": 101.7, "product": "NC1CCN(CC1)C(=O)C1=NC(=C2N=CN(C2=N1)[C@H]1[C@@H]([C@@H]([C@H](O1)C(=O)NCC)O)O)NCC(C1=CC=CC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of (2S,3S,4R,5R)-5-[6-[(2,2-diphenylethyl)amino]-2-({4-[(trifluoroacetyl)amino]-1-piperidinyl}carbonyl)-9H-purin-9-yl]-N-ethyl-3,4-dihydroxytetrahydro-2-furancarboxamide (Preparation 40) (40 mg, 0.056 mmol) in methanol (1 ml) and concentrated aqueous ammonia solution (0.5 ml) was stirred at room temperature ...
10.6084/m9.figshare.5104873.v1
null
Trifluoro group.Secondary amide
Primary amine
null
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CC[NH]CC1
Other
CO.N
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(NC(=O)C(F)(F)F)CC4)nc32)[C@H](O)[C@@H]1O>CO.N>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)N4CCC(N)CC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ba80cd99dcf648b8a14595a793d5c94d
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(N)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.II>>CCNC(=O)C1OC(n2cnc3c(Cl)nc(I)nc32)C(OC(=O)c2ccccc2)C1OC(=O)c1ccccc1
N(=O)OCCCC.C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)Cl)N.II.ICI>>C(C1=CC=CC=C1)(=O)OC1C(OC(C1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)Cl)I
N[c:16]1[n:15][c:13]([Cl:14])[c:12]2[n:11][cH:10][n:9]([C@@H:8]3[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:30]([O:31][C:32](=[O:33])[c:34]4[cH:35][cH:36][cH:37][cH:38][cH:39]4)[C@H:20]3[O:21][C:22](=[O:23])[c:24]3[cH:25][cH:26][cH:27][cH:28][cH:29]3)[c:19]2[n:18]1.I[I:17]>>[CH3:1][CH2:2][NH:3][C:4](=[O:5])[CH...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(N)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.II
CCNC(=O)C1OC(n2cnc3c(Cl)nc(I)nc32)C(OC(=O)c2ccccc2)C1OC(=O)c1ccccc1
null
[Cu]I
C1CCOC1
Functional Group Interconversion
OtherReaction
f2bfbdf2f4ec84bc795fc5810844800ef4e28ee754bf1d46d7f44827ba3d48eb
9c224743a26d9e1c3135e4817dd611aec414d8ea156f02200a3aef865be78b01
O=C(OC1COC(n2cnc3cncnc32)C1OC(=O)c1ccccc1)c1ccccc1
I-[I;H0;D1;+0:1].N-[c;H0;D3;+0:2]1:[#7;a:3]:[c:4]:[c:5]2:[#7;a:6]:[c:7]:[#7;a:8](-[C:9]-[#8:10]):[c:11]:2:[#7;a:12]:1>>[#8:10]-[C:9]-[#7;a:8]1:[c:7]:[#7;a:6]:[c:5]2:[c:4]:[#7;a:3]:[c;H0;D3;+0:2](-[I;H0;D1;+0:1]):[#7;a:12]:[c:11]:1:2
78
[{"value": 78.0, "product": "C(C1=CC=CC=C1)(=O)OC1C(OC(C1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)Cl)I", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.6, "product": "C(C1=CC=CC=C1)(=O)OC1C(OC(C1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)Cl)I", "details": "CALCULATEDPERCENTYIELD", "is_desired":...
null
null
null
null
n-Butyl nitrite (4.65 ml, 39.7 mmol) was added to a suspension of (2R,3R,4S,5S)-2-(2-amino-6-chloro-9H-purin-9-yl)-4-(benzoyloxy)-5-[(ethylamino)carbonyl]-tetrahydro-3-furanyl benzoate (Preparation 46) (8.10 g, 14.7 mmol), iodine (3.73 g, 14.7 mmol), copper(1) iodide (6.16 g, 32.3 mmol) and diiodomethane (12.55 ml, 155...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Aromatic halide
c1ncc2[nH]cnc2n1
c1ncc2nc[nH]c2n1
C1CCOC1.c1ncc2nc[nH]c2n1.c1ccccc1.c1ccccc1
HI
[Cu]I.C1CCOC1
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(N)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.II>[Cu]I.C1CCOC1>CCNC(=O)C1OC(n2cnc3c(Cl)nc(I)nc32)C(OC(=O)c2ccccc2)C1OC(=O)c1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-66fb887f20564c55b3dca39be042d84e
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.Cc1cccc(C(CN)c2cccc(C)c2)c1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4cccc(C)c4)c4cccc(C)c4)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1
C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)Cl)I.CC=1C=C(C=CC1)C(CN)C1=CC(=CC=C1)C>>C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC(=CC=C1)C)C1=CC(=CC=C1)C)I
Cl[c:13]1[c:12]2[n:11][cH:10][n:9]([C@@H:8]3[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:46]([O:47][C:48](=[O:49])[c:50]4[cH:51][cH:52][cH:53][cH:54][cH:55]4)[C@H:36]3[O:37][C:38](=[O:39])[c:40]3[cH:41][cH:42][cH:43][cH:44][cH:45]3)[c:35]2[n:34][c:32]([I:33])[n:31]1.[NH2:14][CH2:15][CH:16]([c:17]1[cH:18][cH:19]...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.Cc1cccc(C(CN)c2cccc(C)c2)c1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4cccc(C)c4)c4cccc(C)c4)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1
null
null
C(C)(C)O
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
d29b1bab4afefe0db66c5d87d4d37a8be0c49cfdb04c6c8844dee54b4b5d425a
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C(O[C@H]1[C@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)ncnc32)OC[C@H]1OC(=O)c1ccccc1)c1ccccc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[I;D1;H0:4]):[#7;a:5]:[c:6]2:[#7;a:7](-[C:8]-[#8:9]):[c:10]:[#7;a:11]:[c:12]:2:1.[C:13]-[C:14]-[NH2;D1;+0:15]>>[#8:9]-[C:8]-[#7;a:7]1:[c:10]:[#7;a:11]:[c:12]2:[c:6]:1:[#7;a:5]:[c:3](-[I;D1;H0:4]):[#7;a:2]:[c;H0;D3;+0:1]:2-[NH;D2;+0:15]-[C:14]-[C:13]
87
[{"value": 87.0, "product": "C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC(=CC=C1)C)C1=CC(=CC=C1)C)I", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.5, "product": "C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=N...
null
null
null
null
A solution of ((2R,3R,4S,5S)-4-(benzoyloxy)-2-(6-chloro-2-iodo-9H-purin-9-yl)-5-[(ethylamino)carbonyl]-tetrahydro-3-furanyl benzoate (Preparation 47) (0.6 g, 0.91 mmol) and 2,2-bis(3-methylphenyl)ethylamine (0.3 g, 1.36 mmol) in isopropanol (20 ml) was stirred at room temperature for 48 hours. Solvent was removed under...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ncc2[nH]cnc2n1
c1ncc2nc[nH]c2n1
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.c1ccccc1.c1ccccc1
HCl
C(C)(C)O
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.Cc1cccc(C(CN)c2cccc(C)c2)c1>C(C)(C)O>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4cccc(C)c4)c4cccc(C)c4)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-86a4871f3cc54886bc9591203388cc9b
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.NCC(c1cccc(Cl)c1)c1cccc(Cl)c1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4cccc(Cl)c4)c4cccc(Cl)c4)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1
C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)Cl)I.ClC=1C=C(C=CC1)C(CN)C1=CC(=CC=C1)Cl>>C(C1=CC=CC=C1)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C1=CC=CC=C1)=O)C(=O)NCC)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC(=CC=C1)Cl)C1=CC(=CC=C1)Cl)I
Cl[c:13]1[c:12]2[n:11][cH:10][n:9]([C@@H:8]3[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:46]([O:47][C:48](=[O:49])[c:50]4[cH:51][cH:52][cH:53][cH:54][cH:55]4)[C@H:36]3[O:37][C:38](=[O:39])[c:40]3[cH:41][cH:42][cH:43][cH:44][cH:45]3)[c:35]2[n:34][c:32]([I:33])[n:31]1.[NH2:14][CH2:15][CH:16]([c:17]1[cH:18][cH:19]...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.NCC(c1cccc(Cl)c1)c1cccc(Cl)c1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4cccc(Cl)c4)c4cccc(Cl)c4)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
d29b1bab4afefe0db66c5d87d4d37a8be0c49cfdb04c6c8844dee54b4b5d425a
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C(O[C@H]1[C@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)ncnc32)OC[C@H]1OC(=O)c1ccccc1)c1ccccc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[I;D1;H0:4]):[#7;a:5]:[c:6]2:[#7;a:7](-[C:8]-[#8:9]):[c:10]:[#7;a:11]:[c:12]:2:1.[C:13]-[C:14]-[NH2;D1;+0:15]>>[#8:9]-[C:8]-[#7;a:7]1:[c:10]:[#7;a:11]:[c:12]2:[c:6]:1:[#7;a:5]:[c:3](-[I;D1;H0:4]):[#7;a:2]:[c;H0;D3;+0:1]:2-[NH;D2;+0:15]-[C:14]-[C:13]
null
[]
null
null
null
null
Prepared from ((2R,3R,4S,5S)-4-(benzoyloxy)-2-(6-chloro-2-iodo-9H-purin-9-yl)-5-[(ethylamino)carbonyl]-tetrahydro-3-furanyl benzoate (Preparation 47) and 2,2-bis(3-chlorophenyl)ethylamine by the same method as Preparation 48. The title compound was obtained as a yellow foam. Conditions: See reaction.notes.procedure_det...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ncc2[nH]cnc2n1
c1ncc2nc[nH]c2n1
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.c1ccccc1.c1ccccc1
HCl
null
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(Cl)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1.NCC(c1cccc(Cl)c1)c1cccc(Cl)c1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4cccc(Cl)c4)c4cccc(Cl)c4)nc(I)nc32)[C@H](OC(=O)c2ccccc2)[C@@H]1OC(=O)c1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1eb4ad4101bd408cab4df1eea911d020
CC(C)N(CCNC(=O)n1ccnc1)C(C)C.NCCNC(=O)OCc1ccccc1>>CC(C)N(CCNC(=O)NCCNC(=O)OCc1ccccc1)C(C)C
Cl.NCCNC(OCC1=CC=CC=C1)=O.C(C)(C)N(CCNC(=O)N1C=NC=C1)C(C)C.C(C)N(CC)CC>>C(C)(C)N(CCNC(=O)NCCNC(OCC1=CC=CC=C1)=O)C(C)C
c1cn([C:8]([NH:7][CH2:6][CH2:5][N:4]([CH:2]([CH3:1])[CH3:3])[CH:24]([CH3:25])[CH3:26])=[O:9])cn1.[NH2:10][CH2:11][CH2:12][NH:13][C:14](=[O:15])[O:16][CH2:17][c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1>>[CH3:1][CH:2]([CH3:3])[N:4]([CH2:5][CH2:6][NH:7][C:8](=[O:9])[NH:10][CH2:11][CH2:12][NH:13][C:14](=[O:15])[O:16][CH2:1...
CC(C)N(CCNC(=O)n1ccnc1)C(C)C.NCCNC(=O)OCc1ccccc1
CC(C)N(CCNC(=O)NCCNC(=O)OCc1ccccc1)C(C)C
null
null
ClCCl
Acylation
OtherReaction
2fca1e60b30bb25dd42d9c3a0a409c10e22201738c1a0d1497c17610c9a7f90b
11d83d172c98dee16e5582fbe84e86af1814ed957a762275a38224e82e89f00a
c1ccccc1
[C:1]-[#7:2]-[C;H0;D3;+0:3](=[O;D1;H0:4])-n1:c:c:n:c:1.[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:5]-[C:6]-[NH;D2;+0:7]-[C;H0;D3;+0:3](=[O;D1;H0:4])-[#7:2]-[C:1]
109.6
[{"value": 109.6, "product": "C(C)(C)N(CCNC(=O)NCCNC(OCC1=CC=CC=C1)=O)C(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of benzyl 2-aminoethylcarbamate hydrochloride (4.33 g, 18.8 mmol), N-[2-(diisopropylamino)ethyl]-1H-imidazole-1-carboxamide (Preparation 19) (3.73 g, 15.64 mmol) and triethylamine (2.62 ml, 18.8 mmol) in dichloromethane (100 ml) was heated under reflux for 14 hours. The solution was allowed to cool to room t...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Primary amine
Urea
c1c[nH]cn1
null
c1ccccc1
Other
ClCCl
null
null
CC(C)N(CCNC(=O)n1ccnc1)C(C)C.NCCNC(=O)OCc1ccccc1>ClCCl>CC(C)N(CCNC(=O)NCCNC(=O)OCc1ccccc1)C(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a9cf39217da648449b967ed86fbe87b0
NCCNC(=O)OCc1ccccc1.O=C(NCCN1CCCCC1)n1ccnc1>>O=C(NCCNC(=O)OCc1ccccc1)NCCN1CCCCC1
Cl.NCCNC(OCC1=CC=CC=C1)=O.N1(CCCCC1)CCNC(=O)N1C=NC=C1>>N1(CCCCC1)CCNC(=O)NCCNC(OCC1=CC=CC=C1)=O
[NH2:3][CH2:4][CH2:5][NH:6][C:7](=[O:8])[O:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1.c1cn([C:2](=[O:1])[NH:17][CH2:18][CH2:19][N:20]2[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]2)cn1>>[O:1]=[C:2]([NH:3][CH2:4][CH2:5][NH:6][C:7](=[O:8])[O:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[NH:17][CH2:18][CH2:...
NCCNC(=O)OCc1ccccc1.O=C(NCCN1CCCCC1)n1ccnc1
O=C(NCCNC(=O)OCc1ccccc1)NCCN1CCCCC1
null
null
null
Acylation
OtherReaction
2fca1e60b30bb25dd42d9c3a0a409c10e22201738c1a0d1497c17610c9a7f90b
11d83d172c98dee16e5582fbe84e86af1814ed957a762275a38224e82e89f00a
O=C(NCCNC(=O)OCc1ccccc1)NCCN1CCCCC1
[C:1]-[#7:2]-[C;H0;D3;+0:3](=[O;D1;H0:4])-n1:c:c:n:c:1.[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:1]-[#7:2]-[C;H0;D3;+0:3](=[O;D1;H0:4])-[NH;D2;+0:7]-[C:6]-[C:5]
null
[]
null
null
null
null
Prepared from benzyl 2-aminoethylcarbamate hydrochloride and N-[2-(1-piperidinyl)ethyl]-1H-imidazole-1-carboxamide (Preparation 18) by a similar procedure to Preparation 50. The title compound was obtained as a yellow oil. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Primary amine
Urea
c1c[nH]cn1
null
c1ccccc1.C1CC[NH]CC1
Other
null
null
null
NCCNC(=O)OCc1ccccc1.O=C(NCCN1CCCCC1)n1ccnc1>>O=C(NCCNC(=O)OCc1ccccc1)NCCN1CCCCC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4a6dcdf464c440f5b2372f95897642bd
CC(C)N(CCNC(=O)NCCNC(=O)OCc1ccccc1)C(C)C>>CC(C)N(CCNC(=O)NCCN)C(C)C.N
C(C)(C)N(CCNC(=O)NCCNC(OCC1=CC=CC=C1)=O)C(C)C>>N.NCCNC(=O)NCCN(C(C)C)C(C)C
O=C(OCc1ccccc1)[NH:13][CH2:12][CH2:11][NH:10][C:8]([NH:7][CH2:6][CH2:5][N:4]([CH:2]([CH3:1])[CH3:3])[CH:14]([CH3:15])[CH3:16])=[O:9]>>[CH3:1][CH:2]([CH3:3])[N:4]([CH2:5][CH2:6][NH:7][C:8](=[O:9])[NH:10][CH2:11][CH2:12][NH2:13])[CH:14]([CH3:15])[CH3:16].[NH3:17]
CC(C)N(CCNC(=O)NCCNC(=O)OCc1ccccc1)C(C)C
CC(C)N(CCNC(=O)NCCN)C(C)C.N
null
[OH-].[Pd+2].[OH-]
C(C)O
Miscellaneous
Hydrogenolysis of amides/imides/carbamates
8432fba507068d7cbb736b1152500b311a95cf832573d00d78ba81d73ce8e2b1
70d56c35a1f2712eddb71d4ede83e11ec1c1a0860c8c4220cbdc53cc816a7d45
null
O=C(-O-C-c1:c:c:c:c:c:1)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
216.3
[{"value": 216.3, "product": "NCCNC(=O)NCCN(C(C)C)C(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of benzyl 2-[({[2-(diisopropylamino)ethyl]amino}carbonyl)amino]ethylcarbamate (Preparation 50) (6.25 g, 14.45 mmol) in ethanol (100 ml) was hydrogenated at room temperature over palladium (II) hydroxide (250 mg) for 4 hours at 414 KPa. The catalyst was removed by filtration through Arbocel (trade mark) and s...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether
Primary amine
c1ccccc1
null
null
HO-
[OH-].[Pd+2].[OH-].C(C)O
null
null
CC(C)N(CCNC(=O)NCCNC(=O)OCc1ccccc1)C(C)C>[OH-].[Pd+2].[OH-].C(C)O>CC(C)N(CCNC(=O)NCCN)C(C)C.N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ea1168c8fcc44c3d867e3ceb3fe2d073
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O.O=C(OCc1ccccc1)c1ccc(CNC(=O)n2ccnc2)cc1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCc4ccc(C(=O)OCc5ccccc5)cc4)nc32)[C@H](O)[C@@H]1O
NCCNC(=O)C1=NC(=C2N=CN(C2=N1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)NCC(C1=CC=CC=C1)C1=CC=CC=C1.N1(C=NC=C1)C(=O)NCC1=CC=C(C(=O)OCC2=CC=CC=C2)C=C1>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NCC1=CC=C(C(=O)OCC2=CC=CC=C2)C=C1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1
[CH3:1][CH2:2][NH:3][C:4](=[O:5])[C@H:6]1[O:7][C@@H:8]([n:9]2[cH:10][n:11][c:12]3[c:13]([NH:14][CH2:15][CH:16]([c:17]4[cH:18][cH:19][cH:20][cH:21][cH:22]4)[c:23]4[cH:24][cH:25][cH:26][cH:27][cH:28]4)[n:29][c:30]([C:31](=[O:32])[NH:33][CH2:34][CH2:35][NH2:36])[n:57][c:58]23)[C@H:59]([OH:60])[C@@H:61]1[OH:62].c1cn([C:37]...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O.O=C(OCc1ccccc1)c1ccc(CNC(=O)n2ccnc2)cc1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCc4ccc(C(=O)OCc5ccccc5)cc4)nc32)[C@H](O)[C@@H]1O
null
null
null
Acylation
OtherReaction
2fca1e60b30bb25dd42d9c3a0a409c10e22201738c1a0d1497c17610c9a7f90b
11d83d172c98dee16e5582fbe84e86af1814ed957a762275a38224e82e89f00a
O=C(NCCNC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@H]3CCCO3)c2n1)NCc1ccc(C(=O)OCc2ccccc2)cc1
[C:1]-[#7:2]-[C;H0;D3;+0:3](=[O;D1;H0:4])-n1:c:c:n:c:1.[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:5]-[C:6]-[NH;D2;+0:7]-[C;H0;D3;+0:3](=[O;D1;H0:4])-[#7:2]-[C:1]
null
[]
null
null
null
null
Prepared from N-(2-aminoethyl)-6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxamide (Preparation 10) and benzyl 4-{[(1H-imidazol-1-ylcarbonyl)amino]methyl}benzoate (Preparation 54) by a similar method to Example 1. The target compound was obta...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Primary amine
Urea
c1c[nH]cn1
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.c1ccccc1.c1ccccc1
Other
null
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O.O=C(OCc1ccccc1)c1ccc(CNC(=O)n2ccnc2)cc1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCc4ccc(C(=O)OCc5ccccc5)cc4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-511b94495bbc4410b949c19d4a59e5c2
CCO.Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
C(C)O.ClC1=NC(=C2N=CN(C2=N1)C1OCCCC1)NCC(C1=CC=CC=C1)C1=CC=CC=C1.C(C)O.C([O-])([O-])=O.[Na+].[Na+]>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)OCC)C1OCCCC1)C1=CC=CC=C1
[CH3:1][CH2:2][OH:3].Cl[c:6]1[n:7][c:8]([NH:9][CH2:10][CH:11]([c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)[c:24]2[n:25][cH:26][n:27]([CH:28]3[CH2:29][CH2:30][CH2:31][CH2:32][O:33]3)[c:34]2[n:35]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[n:7][c:8]([NH:9][CH2:10][CH:11]([c:12]2[...
CCO.Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)P([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2]
null
Acylation
OtherReaction
82ad05ac461299fab6df2807d08ffbf3c3ee8a6a8331beed81410054880ae078
cb2457ddc31be6a34efcab473e76115982b4ecde38288b80cb0e3a124b5c7fdd
c1ccc(C(CNc2ncnc3c2ncn3C2CCCCO2)c2ccccc2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]2:[#7;a:4](-[C:5]-[#8:6]):[c:7]:[#7;a:8]:[c:9]:2:[c:10]:[#7;a:11]:1.[C;D1;H3:12]-[C:13]-[OH;D1;+0:14]>>[#8:6]-[C:5]-[#7;a:4]1:[c:7]:[#7;a:8]:[c:9]2:[c:10]:[#7;a:11]:[c;H0;D3;+0:1](-[C:15](=[O;D1;H0:16])-[O;H0;D2;+0:14]-[C:13]-[C;D1;H3:12]):[#7;a:2]:[c:3]:1:2
null
[]
60
CELSIUS
10
HOUR
To a suspension of palladium (II) acetate (1.50 g, 0.00668 moles) in absolute ethanol (1000 ml) was added 1,1′-bis(diphenylphosphino)ferrocene (7.00 g, 0.0126 moles) and the resultant suspension was stirred under an atmosphere of nitrogen for 18 hours to give the catalyst mixture. To a mixture of 2-chloro-N-(2,2-diphen...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ester
c1ncc2[nH]cnc2n1
c1ncc2[nH]cnc2n1
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOCC1
HCl
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)P([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2]
60
10
CCO.Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C1(=CC=CC=C1)P([C-]1C=CC=C1)C1=CC=CC=C1.[C-]1(C=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Fe+2]>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-81c01a4908cd47028c7b6659b5d734b4
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)OCC)C1OCCCC1)C1=CC=CC=C1.FC(C(=O)O)(F)F>>C1(=CC=CC=C1)C(CNC1=C2N=CNC2=NC(=N1)C(=O)OCC)C1=CC=CC=C1
C1CCC([n:27]2[cH:26][n:25][c:24]3[c:8]([NH:9][CH2:10][CH:11]([c:12]4[cH:13][cH:14][cH:15][cH:16][cH:17]4)[c:18]4[cH:19][cH:20][cH:21][cH:22][cH:23]4)[n:7][c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[n:29][c:28]32)OC1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[n:7][c:8]([NH:9][CH2:10][CH:11]([c:12]2[cH:13][cH:14][cH:15][cH:16][...
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
null
null
C(C)O
Reduction
OtherReaction
5884540ddb12ce381424fd4d8168e9c573ef97adf4e044c59506f6d05225a030
84394d34c591024a84d9393eb3e8adb8ada5a6225c3abafc4dae9aedd4568be4
c1ccc(C(CNc2ncnc3[nH]cnc23)c2ccccc2)cc1
[#8:1]-[C:2](=[O;D1;H0:3])-[c:4]1:[#7;a:5]:[c:6]2:[c:7](:[#7;a:8]:[c:9]:[n;H0;D3;+0:10]:2-C2-C-C-C-C-O-2):[c:11]:[#7;a:12]:1>>[#8:1]-[C:2](=[O;D1;H0:3])-[c:4]1:[#7;a:5]:[c:6]2:[nH;D2;+0:10]:[c:9]:[#7;a:8]:[c:7]:2:[c:11]:[#7;a:12]:1
100.6
[{"value": 100.6, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CNC2=NC(=N1)C(=O)OCC)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a suspension of ethyl 6-[(2,2-diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2-carboxylate (Preparation 62) (250 g, 0.530 moles) in absolute ethanol (1250 ml) under an atmosphere of nitrogen was added trifluoroacetic acid (73.5 g, 0.645 moles) and the resultant mixture was heated at 50° C. for 20 hours....
10.6084/m9.figshare.5104873.v1
null
Ether
null
C1CCOCC1.c1ncc2nc[nH]c2n1
c1ncc2[nH]cnc2n1
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1
HO-
C(C)O
null
null
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>C(C)O>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-24077634027d402792edb18726eda7e5
CC(=O)OC[C@H]1O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]1OC(C)=O.CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1>>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1
FC(S(=O)(=O)O[Si](C)(C)C)(F)F.C(C)(=O)O[C@H]1[C@H](OC(C)=O)[C@H](OC(C)=O)[C@H](O1)COC(C)=O.C([O-])(O)=O.[Na+].CN1CCOCC1.C1(=CC=CC=C1)C(CNC1=C2N=CNC2=NC(=N1)C(=O)OCC)C1=CC=CC=C1>>C(C)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C)=O)COC(C)=O)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OCC
CC(=O)O[C@@H:28]1[O:29][C@H:30]([CH2:31][O:32][C:33]([CH3:34])=[O:35])[C@@H:36]([O:37][C:38]([CH3:39])=[O:40])[C@H:41]1[O:42][C:43]([CH3:44])=[O:45].[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[n:7][c:8]([NH:9][CH2:10][CH:11]([c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)[c:24]2[n:25...
CC(=O)OC[C@H]1O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]1OC(C)=O.CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1
null
null
C(C)(=O)OCC.COCCOC
Heteroatom Alkylation and Arylation
OtherReaction
a90222e67a4a22678b87b59d1ecec052c8245214c445cc6a40c830f6056425a0
555d70919b361b350c80f46e885ff5cda87616c212c907f1056db36bb1eb2375
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
C-C(=O)-O-[C@@H;D3;+0:1]1-[#8:2]-[C:3]-[C:4]-[C:5]-1-[#8:6]-[C:7](-[C;D1;H3:8])=[O;D1;H0:9].[#8:10]-[C:11](=[O;D1;H0:12])-[c:13]1:[#7;a:14]:[c:15]2:[nH;D2;+0:16]:[c:17]:[#7;a:18]:[c:19]:2:[c:20]:[#7;a:21]:1>>[#8:10]-[C:11](=[O;D1;H0:12])-[c:13]1:[#7;a:14]:[c:15]2:[c:19](:[#7;a:18]:[c:17]:[n;H0;D3;+0:16]:2-[C@@H;D3;+0:1...
null
[]
55
CELSIUS
null
null
To a suspension of ethyl 6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 63) (40.0 g, 0.103 moles) in anhydrous 1,2-dimethoxyethane (240 ml) under an atmosphere of nitrogen was added 4-methylmorpholine (11.5 g, 12.5 ml, 0.114 moles) and the resultant mixture was heated to 45° C. with stirring. To this...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether
Ether
C1CCOC1.c1ncc2[nH]cnc2n1
c1ncc2[nH]cnc2n1.C1CCOC1
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOC1
HO-
C(C)(=O)OCC.COCCOC
55
null
CC(=O)OC[C@H]1O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]1OC(C)=O.CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1>C(C)(=O)OCC.COCCOC>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f2a6a459e69e4f6da6d4623423fcd8a8
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1>>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
C(C)(=O)O.C(C)(=O)O[C@H]1[C@@H](O[C@@H]([C@H]1OC(C)=O)COC(C)=O)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OCC.[O-]CC.[Na+]>>O[C@H]1[C@@H](O[C@@H]([C@H]1O)CO)N1C2=NC(=NC(=C2N=C1)NCC(C1=CC=CC=C1)C1=CC=CC=C1)C(=O)OCC
CC(=O)[O:32][CH2:31][C@H:30]1[O:29][C@@H:28]([n:27]2[cH:26][n:25][c:24]3[c:8]([NH:9][CH2:10][CH:11]([c:12]4[cH:13][cH:14][cH:15][cH:16][cH:17]4)[c:18]4[cH:19][cH:20][cH:21][cH:22][cH:23]4)[n:7][c:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[n:38][c:37]32)[C@H:35]([O:36]C(C)=O)[C@@H:33]1[O:34]C(C)=O>>[CH3:1][CH2:2][O:3][C:4](=[...
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
null
null
C(C)O
Reduction
OtherReaction
b1205f31a625dd524c4abcf6ea407c1a38966308677d8535d59411f69b7afe49
53784a05a6c1858c11deb702d4a1392e7852c783da9a57d4771755f87682c932
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
C-C(=O)-[O;H0;D2;+0:1]-[C:2]-[C:3]1-[#8:4]-[C:5]-[C:6](-[O;H0;D2;+0:7]-C(-C)=O)-[C:8]-1-[O;H0;D2;+0:9]-C(-C)=O>>[OH;D1;+0:1]-[C:2]-[C:3]1-[#8:4]-[C:5]-[C:6](-[OH;D1;+0:7])-[C:8]-1-[OH;D1;+0:9]
null
[]
null
null
null
null
To a solution of crude ethyl 9-{(2R,3R,4R,5R)-3,4-bis(acetyloxy)-5-[(acetyloxy)methyl]tetrahydro-2-furanyl}-6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 64) (74.9 g, assumed 0.103 moles) in warm absolute ethanol (330 ml) was added sodium ethoxide (1.2 g, 0.018 moles) in portions over 23 hours. The ...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Ester
Primary alcohol.Secondary alcohol.Secondary alcohol
null
null
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOC1
HO-
C(C)O
null
null
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](COC(C)=O)[C@@H](OC(C)=O)[C@H]3OC(C)=O)c2n1>C(C)O>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@@H](O)[C@H]3O)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c861fea8709446249bd3147edec32b75
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@H]4OC(C)(C)O[C@H]43)c2n1>>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](C(=O)O)[C@H]4OC(C)(C)O[C@H]43)c2n1
Cl.OC[C@H]1O[C@H]([C@H]2[C@@H]1OC(O2)(C)C)N2C1=NC(=NC(=C1N=C2)NCC(C2=CC=CC=C2)C2=CC=CC=C2)C(=O)OCC.P(=O)(O)(O)[O-].[Na+].Cl(=O)[O-].[Na+].S(=O)([O-])[O-].[Na+].[Na+]>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)OCC)[C@@H]1O[C@@H]([C@@H]2[C@H]1OC(O2)(C)C)C(=O)O)C2=CC=CC=C2
[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[n:7][c:8]([NH:9][CH2:10][CH:11]([c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)[c:24]2[n:25][cH:26][n:27]([C@@H:28]3[O:29][C@H:30]([CH2:31][OH:33])[C@H:34]4[O:35][C:36]([CH3:37])([CH3:38])[O:39][C@@H:40]34)[c:41]2[n:42]1>>[CH3:1][CH2:2][O:3...
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@H]4OC(C)(C)O[C@H]43)c2n1
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](C(=O)O)[C@H]4OC(C)(C)O[C@H]43)c2n1
null
Cl[O-].[Na+]
O.C(C)#N
Oxidation
Oxidation of alcohol to carboxylic acid
b709baac44a995a9a8f6386a6b5d87f98c32eb5a0636340abc1f778fae827230
4454822e22dc2dc24e7495385256bfce456e337c240bb764261f81dbeda1aaa1
c1ccc(C(CNc2ncnc3c2ncn3[C@@H]2OC[C@H]3OCO[C@@H]23)c2ccccc2)cc1
[#8:1]-[C:2]-[C:3](-[CH2;D2;+0:4]-[O;D1;H1:5])-[#8:6]-[C:7]>>[#8:1]-[C:2]-[C:3](-[C;H0;D3;+0:4](=[O;D1;H0:8])-[O;D1;H1:5])-[#8:6]-[C:7]
null
[]
null
null
18
HOUR
To a solution of ethyl 9-[(3aR,4R,6R,6aR)-6-(hydroxymethyl)-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl]-6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 66) (15.4 g, 0.0276 moles) in acetonitrile under an atmosphere of nitrogen was added 2,2,6,6-tetramethylpiperidinyl-1-oxy, free radical (0.30 g...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Carboxylic acid
null
null
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1O[C@H]2COC[C@H]2O1
Other
Cl[O-].[Na+].O.C(C)#N
null
18
CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](CO)[C@H]4OC(C)(C)O[C@H]43)c2n1>Cl[O-].[Na+].O.C(C)#N>CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](C(=O)O)[C@H]4OC(C)(C)O[C@H]43)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-347e3b4fbd954295861786e00cfc0e34
CCN.CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](C(=O)O)[C@H]4OC(C)(C)O[C@H]43)c2n1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OCC)nc32)[C@@H]2OC(C)(C)O[C@@H]21
C(C)N.C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)OCC)[C@@H]1O[C@@H]([C@@H]2[C@H]1OC(O2)(C)C)C(=O)O)C2=CC=CC=C2.C(=O)(N1C=NC=C1)N1C=NC=C1.C(C)N.O>>C(C)NC(=O)[C@H]1O[C@H]([C@H]2[C@@H]1OC(O2)(C)C)N2C1=NC(=NC(=C1N=C2)NCC(C2=CC=CC=C2)C2=CC=CC=C2)C(=O)OCC
[CH3:1][CH2:2][NH2:3].O[C:4](=[O:5])[C@H:6]1[O:7][C@@H:8]([n:9]2[cH:10][n:11][c:12]3[c:13]([NH:14][CH2:15][CH:16]([c:17]4[cH:18][cH:19][cH:20][cH:21][cH:22]4)[c:23]4[cH:24][cH:25][cH:26][cH:27][cH:28]4)[n:29][c:30]([C:31](=[O:32])[O:33][CH2:34][CH3:35])[n:36][c:37]23)[C@@H:38]2[O:39][C:40]([CH3:41])([CH3:42])[O:43][C@H...
CCN.CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](C(=O)O)[C@H]4OC(C)(C)O[C@H]43)c2n1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OCC)nc32)[C@@H]2OC(C)(C)O[C@@H]21
null
null
O1CCCC1
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
c1ccc(C(CNc2ncnc3c2ncn3[C@@H]2OC[C@H]3OCO[C@@H]23)c2ccccc2)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[#8:4]-[C:5])-[C:6]-[#8:7].[C;D1;H3:8]-[C:9]-[NH2;D1;+0:10]>>[#8:7]-[C:6]-[C:3](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:10]-[C:9]-[C;D1;H3:8])-[#8:4]-[C:5]
78.9
[{"value": 78.9, "product": "C(C)NC(=O)[C@H]1O[C@H]([C@H]2[C@@H]1OC(O2)(C)C)N2C1=NC(=NC(=C1N=C2)NCC(C2=CC=CC=C2)C2=CC=CC=C2)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
15
CELSIUS
2
HOUR
To a solution of (3aS,4S,6R,6aR)-6-[6-[(2,2-diphenylethyl)amino]-2-(ethoxycarbonyl)-9H-purin-9-yl]-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxole-4-carboxylic acid (Preparations 67 and 68) (20.0 g, 0.0349 moles) in anhydrous tetrahydrofuran (100 ml) under an atmosphere of nitrogen was added 1,1′-carbonyldiimidazole (6.8...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1O[C@H]2COC[C@H]2O1
HO-
O1CCCC1
15
2
CCN.CCOC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@@H]3O[C@H](C(=O)O)[C@H]4OC(C)(C)O[C@H]43)c2n1>O1CCCC1>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OCC)nc32)[C@@H]2OC(C)(C)O[C@@H]21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-11f81d031b174a5a8daa77a49c922b63
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OCC)nc32)[C@@H]2OC(C)(C)O[C@@H]21>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@@H]2OC(C)(C)O[C@@H]21
C(C)NC(=O)[C@H]1O[C@H]([C@H]2[C@@H]1OC(O2)(C)C)N2C1=NC(=NC(=C1N=C2)NCC(C2=CC=CC=C2)C2=CC=CC=C2)C(=O)OCC.[OH-].[Na+]>>C(C)NC(=O)[C@H]1O[C@H]([C@H]2[C@@H]1OC(O2)(C)C)N2C1=NC(=NC(=C1N=C2)NCC(C2=CC=CC=C2)C2=CC=CC=C2)C(=O)O
CC[O:33][C:31]([c:30]1[n:29][c:13]([NH:14][CH2:15][CH:16]([c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[c:23]2[cH:24][cH:25][cH:26][cH:27][cH:28]2)[c:12]2[n:11][cH:10][n:9]([C@@H:8]3[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:42]4[C@H:36]3[O:37][C:38]([CH3:39])([CH3:40])[O:41]4)[c:35]2[n:34]1)=[O:32]>>[CH3:1][C...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OCC)nc32)[C@@H]2OC(C)(C)O[C@@H]21
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@@H]2OC(C)(C)O[C@@H]21
null
null
CO
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(C(CNc2ncnc3c2ncn3[C@@H]2OC[C@H]3OCO[C@@H]23)c2ccccc2)cc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4](:[#7;a:5]):[#7;a:6]>>[#7;a:5]:[c:4](-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]):[#7;a:6]
98.8
[{"value": 98.8, "product": "C(C)NC(=O)[C@H]1O[C@H]([C@H]2[C@@H]1OC(O2)(C)C)N2C1=NC(=NC(=C1N=C2)NCC(C2=CC=CC=C2)C2=CC=CC=C2)C(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
To a solution of ethyl 9-{(3aR,4R,6S,6aS)-6-[(ethylamino)carbonyl]-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl}-6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 69) (16.47 g, 0.0274 moles) in methanol (164 ml) was added aqueous sodium hydroxide (30.2 ml of a 1 M solution, 0.0302 moles) and the re...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1O[C@H]2COC[C@H]2O1
Other
CO
null
1.5
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OCC)nc32)[C@@H]2OC(C)(C)O[C@@H]21>CO>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)O)nc32)[C@@H]2OC(C)(C)O[C@@H]21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9de8626dfbfe4853a1c297e1bbb92197
CC(C)(C)OC(=O)NCCN.NC1CCN(c2ccccn2)CC1.O=C(n1ccnc1)n1ccnc1>>CC(C)(C)OC(=O)NCCNC(=O)NC1CCN(c2ccccn2)CC1
NCCNC(OC(C)(C)C)=O.Cl.Cl.N1=C(C=CC=C1)N1CCC(CC1)N.C(=O)(N1C=NC=C1)N1C=NC=C1.C(C)(C)N(C(C)C)CC>>N1=C(C=CC=C1)N1CCC(CC1)NC(=O)NCCNC(OC(C)(C)C)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][NH2:11].[NH2:14][CH:15]1[CH2:16][CH2:17][N:18]([c:19]2[cH:20][cH:21][cH:22][cH:23][n:24]2)[CH2:25][CH2:26]1.c1cn([C:12](n2ccnc2)=[O:13])cn1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][NH:11][C:12](=[O:13])[NH:14][CH:15]1[CH...
CC(C)(C)OC(=O)NCCN.NC1CCN(c2ccccn2)CC1.O=C(n1ccnc1)n1ccnc1
CC(C)(C)OC(=O)NCCNC(=O)NC1CCN(c2ccccn2)CC1
null
null
C(C)#N
Acylation
OtherReaction
4bbb31b0118d7292be8236579c179606942bc7ed40684e26f7727a569ab5c30d
4ff96020857e85930fbee987c7fa4ef615e45b2ea39cff27ceaec8f9174d5b6f
c1ccc(N2CCCCC2)nc1
[C:1]-[C:2](-[NH2;D1;+0:3])-[C:4].[C:5]-[C:6]-[NH2;D1;+0:7].[O;D1;H0:8]=[C;H0;D3;+0:9](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[C:1]-[C:2](-[NH;D2;+0:3]-[C;H0;D3;+0:9](=[O;D1;H0:8])-[NH;D2;+0:7]-[C:6]-[C:5])-[C:4]
null
[]
null
null
20
MINUTE
an ice-cooled solution of 1-(2-pyridinyl)-4-piperidinylamine dihydrochloride EP-A-0021973) (20.82 g, 0.0832 moles) and 1,1′-carbonyldiimidazole (14.85 g, 0.915 moles) in acetonitrile (140 ml) under an atmosphere of nitrogen was added N,N-di-iso-propylethylamine (22.0 g, 29.7 ml, 0.170 moles) over a period of 20 minutes...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Primary amine
Urea
c1c[nH]cn1.c1c[nH]cn1
null
C1CC[NH]CC1.c1ccncc1
Other
C(C)#N
null
0.333333
CC(C)(C)OC(=O)NCCN.NC1CCN(c2ccccn2)CC1.O=C(n1ccnc1)n1ccnc1>C(C)#N>CC(C)(C)OC(=O)NCCNC(=O)NC1CCN(c2ccccn2)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1867737373ad4bb48701270e5edc5939
Cc1cc(C)c(S(=O)(=O)Cl)c(C)c1.NCCCCN>>Cc1cc(C)c(S(=O)(=O)NCCCCNS(=O)(=O)c2c(C)cc(C)cc2C)c(C)c1
C1(=C(C(=CC(=C1)C)C)S(=O)(=O)Cl)C.NCCCCN>>C1(=C(C(=CC(=C1)C)C)S(=O)(=O)NCCCCNS(=O)(=O)C1=C(C=C(C=C1C)C)C)C
Cl[S:7]([c:6]1[c:23]([CH3:24])[cH:22][c:2]([CH3:1])[cH:30][c:28]1[CH3:29])(=[O:8])=[O:9].[CH2:3]([CH2:4][CH2:5][NH2:10])[CH2:14][NH2:15]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([S:7](=[O:8])(=[O:9])[NH:10][CH2:11][CH2:12][CH2:13][CH2:14][NH:15][S:16](=[O:17])(=[O:18])[c:19]2[c:20]([CH3:21])[cH:22][c:23]([CH3:24])[cH:25...
Cc1cc(C)c(S(=O)(=O)Cl)c(C)c1.NCCCCN
Cc1cc(C)c(S(=O)(=O)NCCCCNS(=O)(=O)c2c(C)cc(C)cc2C)c(C)c1
null
null
[OH-].[Na+].C(Cl)Cl
Aromatic Heterocycle Formation
OtherReaction
e4d9d7fc6666959977fbf8132e7d8913fe3ccae568038c3a25f79e909aff7c7c
49e17eef2449ba97ee4819a6ce246acf1c58e3d5b3abe8a2f31d396efdacf84d
O=S(=O)(NCCCCNS(=O)(=O)c1ccccc1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c;H0;D3;+0:4]1:[c:5](-[C;D1;H3:6]):[c:7]:[c;H0;D3;+0:8](-[C;D1;H3:9]):[cH;D2;+0:10]:[c;H0;D3;+0:11]:1-[C;D1;H3:12].[NH2;D1;+0:13]-[CH2;D2;+0:14]-[CH2;D2;+0:15]-[CH2;D2;+0:16]-[CH2;D2;+0:17]-[NH2;D1;+0:18]>>[C;D1;H3:9]-[c;H0;D3;+0:8]1:[c:7]:[c:5](-[C;D1;H3:6]):[c;H0;D3;+0:4...
90
[{"value": 90.0, "product": "C1(=C(C(=CC(=C1)C)C)S(=O)(=O)NCCCCNS(=O)(=O)C1=C(C=C(C=C1C)C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.5, "product": "C1(=C(C(=CC(=C1)C)C)S(=O)(=O)NCCCCNS(=O)(=O)C1=C(C=C(C=C1C)C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
2-Mesitylenesulfonyl chloride (54.40 g, 0.249 mol) in CH2Cl2 (300 ml) was added to 1,4-diaminobutane (11.34 g, 0.129 mol) in 1 N NaOH (300 ml) at 0° C., and the biphasic mixture was stirred for 24 hours at room temperature. Organic solvent was evaporated and 2.4 N HCl (250 ml) was added to the combined portions. Solid ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Primary amine.Sulfonyl halide
Sulfonamide.Sulfonamide
c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
null
[OH-].[Na+].C(Cl)Cl
null
24
Cc1cc(C)c(S(=O)(=O)Cl)c(C)c1.NCCCCN>[OH-].[Na+].C(Cl)Cl>Cc1cc(C)c(S(=O)(=O)NCCCCNS(=O)(=O)c2c(C)cc(C)cc2C)c(C)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dc1fa503d8b442db9694da96e0879be1
Cc1cc(C)c(S(=O)(=O)Cl)c(C)c1.OCCC1CCNCC1>>Cc1cc(C)c(S(=O)(=O)OCCC2CCN(S(=O)(=O)c3c(C)cc(C)cc3C)CC2)c(C)c1
C1(=C(C(=CC(=C1)C)C)S(=O)(=O)Cl)C.N1CCC(CC1)CCO>>CC1=C(C(=CC(=C1)C)C)S(=O)(=O)N1CCC(CC1)CCOS(=O)(=O)C1=C(C=C(C=C1C)C)C
Cl[S:7]([c:6]1[c:24]([CH3:25])[cH:3][c:2]([CH3:1])[cH:32][c:31]1[CH3:5])(=[O:8])=[O:9].[OH:10][CH2:11][CH2:12][CH:13]1[CH2:14][CH2:15][NH:16][CH2:29][CH2:30]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([S:7](=[O:8])(=[O:9])[O:10][CH2:11][CH2:12][CH:13]2[CH2:14][CH2:15][N:16]([S:17](=[O:18])(=[O:19])[c:20]3[c:21]([CH3:22])...
Cc1cc(C)c(S(=O)(=O)Cl)c(C)c1.OCCC1CCNCC1
Cc1cc(C)c(S(=O)(=O)OCCC2CCN(S(=O)(=O)c3c(C)cc(C)cc3C)CC2)c(C)c1
null
null
N1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
3a84d1d118995a3875138345738afc2f77691666e3414ebbb2805c8c9ab26406
336c2018f2656bb6f8a9f916ae1945c5b6aece99517a0b2dd11edeef58f4c413
O=S(=O)(OCCC1CCN(S(=O)(=O)c2ccccc2)CC1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c;H0;D3;+0:4]1:[c;H0;D3;+0:5](-[C;D1;H3:6]):[cH;D2;+0:7]:[c;H0;D3;+0:8](-[C;D1;H3:9]):[cH;D2;+0:10]:[c;H0;D3;+0:11]:1-[CH3;D1;+0:12].[C:13]-[C:14]-[NH;D2;+0:15]-[C:16]-[C:17].[C:18]-[C:19]-[OH;D1;+0:20]>>[C:13]-[C:14]-[N;H0;D3;+0:15](-[#16:21](=[O;D1;H0:22])(=[O;D1;H0:23])...
null
[]
null
null
44
HOUR
2-Mesitylenesulfonyl chloride (24.78 g, 0.113 mol) in pyridine (60 ml) was added all at once to 4-piperidine-ethanol (5.58 g, 43.2 mmol) in pyridine (25 ml) at −16° C.; the temperature rose to −11° C. The flask was stored in the refrigerator at 5.5° C. for 44 hours under argon. The reaction mixture was poured into ice ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Secondary amine.Sulfonyl halide
Tertiary amine.Sulfonate
c1ccccc1.C1CCNCC1
c1ccccc1.C1CC[NH]CC1.c1ccccc1
c1ccccc1.C1CC[NH]CC1.c1ccccc1
null
N1=CC=CC=C1
null
44
Cc1cc(C)c(S(=O)(=O)Cl)c(C)c1.OCCC1CCNCC1>N1=CC=CC=C1>Cc1cc(C)c(S(=O)(=O)OCCC2CCN(S(=O)(=O)c3c(C)cc(C)cc3C)CC2)c(C)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1bb450c743ff480295cb2836392ef9e4
C1=COCCC1.Oc1ccc(I)cc1>>Ic1ccc(OC2CCCCO2)cc1
C=1(C(=CC=CC1)S(=O)(=O)O)C.IC1=CC=C(C=C1)O.O1CCCC=C1>>IC1=CC=C(C=C1)OC1OCCCC1
[CH:7]1=[CH:8][CH2:9][CH2:10][CH2:11][O:12]1.[I:1][c:2]1[cH:3][cH:4][c:5]([OH:6])[cH:13][cH:14]1>>[I:1][c:2]1[cH:3][cH:4][c:5]([O:6][CH:7]2[CH2:8][CH2:9][CH2:10][CH2:11][O:12]2)[cH:13][cH:14]1
C1=COCCC1.Oc1ccc(I)cc1
Ic1ccc(OC2CCCCO2)cc1
null
CC=1C=CC(=CC1)S(=O)(=O)O
C(Cl)Cl
Heteroatom Alkylation and Arylation
oxa-Michael addition
1c7c788bec8addec628516b12629525fab255984248a4af23c71106a7726e25d
da6d2e768f263ce18da31b53a21ee41abe25d00717257e942f83f912a04f86d8
c1ccc(OC2CCCCO2)cc1
[#8:1]1-[C:2]-[C:3]-[C:4]-[CH;D2;+0:5]=[CH;D2;+0:6]-1.[OH;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[c:9]:[c:8](-[O;H0;D2;+0:7]-[CH;D3;+0:6]1-[#8:1]-[C:2]-[C:3]-[C:4]-[CH2;D2;+0:5]-1):[c:10]
92.1
[{"value": 92.0, "product": "IC1=CC=C(C=C1)OC1OCCCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.1, "product": "IC1=CC=C(C=C1)OC1OCCCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
20
CELSIUS
15
MINUTE
To a stirred solution of 4-iodophenol (11.0 g, 50 mmol) in CH2Cl2 (50 ml) cooled with an ice bath, dihydropyran (5.0 g, 60 mmol) was added dropwise over 10 min at 0–5° C. After the solution became clear, toluenesulfonic acid, TsOH, (10 mg) was added. The solution was stirred at 20° C. for 15 min. Then it was quenched b...
10.6084/m9.figshare.5104873.v1
null
Ether.Aromatic alcohol
Ether.Ether
C1=COCCC1
C1CCOCC1
c1ccccc1.C1CCOCC1
null
CC=1C=CC(=CC1)S(=O)(=O)O.C(Cl)Cl
20
0.25
C1=COCCC1.Oc1ccc(I)cc1>CC=1C=CC(=CC1)S(=O)(=O)O.C(Cl)Cl>Ic1ccc(OC2CCCCO2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-eeefb2a199d048a9aeec94c9f646f6f9
C#C[Si](C)(C)C.Ic1ccc(OC2CCCCO2)cc1>>C[Si](C)(C)C#Cc1ccc(OC2CCCCO2)cc1
C[Si](C)(C)C#C.IC1=CC=C(C=C1)OC1OCCCC1>>O1C(CCCC1)OC1=CC=C(C=C1)C#C[Si](C)(C)C
[CH3:1][Si:2]([CH3:3])([CH3:4])[C:5]#[CH:6].I[c:7]1[cH:8][cH:9][c:10]([O:11][CH:12]2[CH2:13][CH2:14][CH2:15][CH2:16][O:17]2)[cH:18][cH:19]1>>[CH3:1][Si:2]([CH3:3])([CH3:4])[C:5]#[C:6][c:7]1[cH:8][cH:9][c:10]([O:11][CH:12]2[CH2:13][CH2:14][CH2:15][CH2:16][O:17]2)[cH:18][cH:19]1
C#C[Si](C)(C)C.Ic1ccc(OC2CCCCO2)cc1
C[Si](C)(C)C#Cc1ccc(OC2CCCCO2)cc1
null
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.[Cu]I
C(C)(C)NC(C)C
C-C Coupling
Sonogashira alkyne_aryl halide
15c08902746c61a960c314898ce6bb5fcc5e189f9e057388c59dba9ec9d0c81c
305eca0fd2975da49e7f69e4edfb9dc1cbce82513954bc5a73be3289e70e5f76
c1ccc(OC2CCCCO2)cc1
I-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[C;D1;H3:6]-[#14:7](-[C;D1;H3:8])(-[C;D1;H3:9])-[C:10]#[CH;D1;+0:11]>>[C;D1;H3:6]-[#14:7](-[C;D1;H3:8])(-[C;D1;H3:9])-[C:10]#[C;H0;D2;+0:11]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
2
HOUR
To a degassed solution of compound 1 (9.12 g, 30 mmol) in diisopropylamine (180 ml) under nitrogen, Pd(PPh3)2Cl2 (140 mg, 0.2 mmol) and CuI (78 mg, 0.4 mmol) were added. Then trimethylsilyl acetylene (3.3 g, 33 mmol) was added dropwise to this clear solution. The reaction mixture was stirred for 2 hours at room tempera...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Alkyne
Alkyne
c1ccccc1
c1ccccc1
c1ccccc1.C1CCOCC1
HI
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.[Cu]I.C(C)(C)NC(C)C
null
2
C#C[Si](C)(C)C.Ic1ccc(OC2CCCCO2)cc1>Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.[Cu]I.C(C)(C)NC(C)C>C[Si](C)(C)C#Cc1ccc(OC2CCCCO2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9f5b87a7370b42dc9bc44c6cfc944008
C[Si](C)(C)C#Cc1ccc(OC2CCCCO2)cc1>>C#Cc1ccc(OC2CCCCO2)cc1
O1C(CCCC1)OC1=CC=C(C=C1)C#C[Si](C)(C)C>>O1C(CCCC1)OC1=CC=C(C=C1)C#C
C[Si](C)(C)[C:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([O:7][CH:8]2[CH2:9][CH2:10][CH2:11][CH2:12][O:13]2)[cH:14][cH:15]1>>[CH:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([O:7][CH:8]2[CH2:9][CH2:10][CH2:11][CH2:12][O:13]2)[cH:14][cH:15]1
C[Si](C)(C)C#Cc1ccc(OC2CCCCO2)cc1
C#Cc1ccc(OC2CCCCO2)cc1
null
null
CO
Deprotection
TMS deprotection from alkyne
e85676bb81da384790c9c858d44f182cdd01e3a79f77f7a239fe38487234cb96
56d526d7c9cb1bd7bee4940e216a9b1dd4597fd025a186b8d6e4675d8f4db26b
c1ccc(OC2CCCCO2)cc1
C-[Si](-C)(-C)-[C;H0;D2;+0:1]#[C:2]-[c:3]>>[CH;D1;+0:1]#[C:2]-[c:3]
null
[]
null
null
4
HOUR
(9.3 g, 160 mmol) was added to a stirred solution of 2 (22.6 g, 80 mmol) in MeOH (150 ml). The reaction mixture was stirred at room temperature for about 4 hours. After the reaction finished (GC shows no starting material remaining), the solvent was removed under reduced pressure on a rotary evaporator. The residue was...
10.6084/m9.figshare.5104873.v1
null
Alkyne.Silyl protective group
Alkyne
null
null
c1ccccc1.C1CCOCC1
Other
CO
null
4
C[Si](C)(C)C#Cc1ccc(OC2CCCCO2)cc1>CO>C#Cc1ccc(OC2CCCCO2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d3dd416e317947b78c70bab9354dfb39
C#Cc1ccc(OC2CCCCO2)cc1.FC(F)(F)c1ccc(Br)cc1>>FC(F)(F)c1ccc(C#Cc2ccc(OC3CCCCO3)cc2)cc1
O1C(CCCC1)OC1=CC=C(C=C1)C#C.BrC1=CC=C(C=C1)C(F)(F)F>>O1C(CCCC1)OC1=CC=C(C=C1)C#CC1=CC=C(C=C1)C(F)(F)F
[CH:9]#[C:10][c:11]1[cH:12][cH:13][c:14]([O:15][CH:16]2[CH2:17][CH2:18][CH2:19][CH2:20][O:21]2)[cH:22][cH:23]1.Br[c:8]1[cH:7][cH:6][c:5]([C:2]([F:1])([F:3])[F:4])[cH:25][cH:24]1>>[F:1][C:2]([F:3])([F:4])[c:5]1[cH:6][cH:7][c:8]([C:9]#[C:10][c:11]2[cH:12][cH:13][c:14]([O:15][CH:16]3[CH2:17][CH2:18][CH2:19][CH2:20][O:21]3...
C#Cc1ccc(OC2CCCCO2)cc1.FC(F)(F)c1ccc(Br)cc1
FC(F)(F)c1ccc(C#Cc2ccc(OC3CCCCO3)cc2)cc1
null
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.[Cu]I
C(C)(C)NC(C)C
C-C Coupling
Sonogashira alkyne_aryl halide
15c08902746c61a960c314898ce6bb5fcc5e189f9e057388c59dba9ec9d0c81c
305eca0fd2975da49e7f69e4edfb9dc1cbce82513954bc5a73be3289e70e5f76
C(#Cc1ccc(OC2CCCCO2)cc1)c1ccccc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[CH;D1;+0:6]#[C:7]-[c:8]>>[c:8]-[C:7]#[C;H0;D2;+0:6]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
80
CELSIUS
2
HOUR
A solution of 3 (12.1 g, 60 mmol) and 4-bromobenzotriflouride (14.85 g, 66 mmol) in diisopropylamine (250 ml) was heated to 30° C. under nitrogen, and the solution was degassed. Then Pd(PPh3)2Cl2 (210 mg, 0.3 mmol) and copper(I) iodide (114 mg, 0.6 mmol) were added to this clear solution. The reaction mixture was stirr...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Alkyne
Alkyne
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1.C1CCOCC1
HBr
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.[Cu]I.C(C)(C)NC(C)C
80
2
C#Cc1ccc(OC2CCCCO2)cc1.FC(F)(F)c1ccc(Br)cc1>Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl.[Cu]I.C(C)(C)NC(C)C>FC(F)(F)c1ccc(C#Cc2ccc(OC3CCCCO3)cc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-001c79b908c44af0b3cbb88ecfd5d8af
FC(F)(F)c1ccc(C#Cc2ccc(OC3CCCCO3)cc2)cc1>>Oc1cccc(C#Cc2ccc(C(F)(F)F)cc2)c1
O1C(CCCC1)OC1=CC=C(C=C1)C#CC1=CC=C(C=C1)C(F)(F)F.C(Cl)Cl.CC=1C=CC(=CC1)S(=O)(=O)O>>OC=1C=CC=C(C1)C#CC1=CC=C(C=C1)C(F)(F)F
C1CCC([O:1][c:2]2[cH:3][cH:19][c:6]([C:7]#[C:8][c:9]3[cH:10][cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17][cH:18]3)[cH:5][cH:4]2)OC1>>[OH:1][c:2]1[cH:3][cH:4][cH:5][c:6]([C:7]#[C:8][c:9]2[cH:10][cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17][cH:18]2)[cH:19]1
FC(F)(F)c1ccc(C#Cc2ccc(OC3CCCCO3)cc2)cc1
Oc1cccc(C#Cc2ccc(C(F)(F)F)cc2)c1
null
null
CO
Miscellaneous
OtherReaction
16dbd123c57e1815d831a6d1b3507538729761040e5fd17321613b472b962401
97b700253a515732e056bebfec7d29d55492867916f45a12199b66c78e6a3460
C(#Cc1ccccc1)c1ccccc1
[c:1]-[C:2]#[C:3]-[c:4]1:[c:5]:[cH;D2;+0:6]:[c;H0;D3;+0:7](-[O;H0;D2;+0:8]-C2-C-C-C-C-O-2):[cH;D2;+0:9]:[cH;D2;+0:10]:1>>[OH;D1;+0:8]-[c;H0;D3;+0:7]1:[cH;D2;+0:10]:[c:4](-[C:3]#[C:2]-[c:1]):[c:5]:[cH;D2;+0:6]:[cH;D2;+0:9]:1
9,057.1
[{"value": 90.0, "product": "OC=1C=CC=C(C1)C#CC1=CC=C(C=C1)C(F)(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 9057.1, "product": "OC=1C=CC=C(C1)C#CC1=CC=C(C=C1)C(F)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
30
CELSIUS
1
HOUR
Coumpound 4 (13.84 g, 40 mmol), CH2Cl2 (75 ml) and MeOH (125 ml) were placed in a 250 ml round bottomed flask, then TsOH (0.4 g, 0.4 mmol) was added. The reaction mixture was stirred at 30° C. for 1 hour. When the reaction was finished (TLC shows no starting material remaining), the solvent was removed by rotary evapor...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Aromatic alcohol
C1CCOCC1.c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HO-
CO
30
1
FC(F)(F)c1ccc(C#Cc2ccc(OC3CCCCO3)cc2)cc1>CO>Oc1cccc(C#Cc2ccc(C(F)(F)F)cc2)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dd33ac29f3d04c6eaaab7d588e3dff45
CCCCOC(=O)c1ccc(N)cc1.N#C[S-].O=C(Cl)c1ccc2ccccc2c1>>CCCCOC(=O)c1ccc(NC(=S)NC(=O)c2ccc3ccccc3c2)cc1
C1=C(C=CC2=CC=CC=C12)C(=O)Cl.[S-]C#N.[NH4+].NC1=CC=C(C(=O)OCCCC)C=C1>>C(CCC)OC(C1=CC=C(C=C1)NC(=S)NC(=O)C1=CC2=CC=CC=C2C=C1)=O
[CH3:1][CH2:2][CH2:3][CH2:4][O:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([NH2:12])[cH:28][cH:29]1.[C:13]([S-:14])#[N:15].Cl[C:16](=[O:17])[c:18]1[cH:19][cH:20][c:21]2[cH:22][cH:23][cH:24][cH:25][c:26]2[cH:27]1>>[CH3:1][CH2:2][CH2:3][CH2:4][O:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=[S:14])[NH:15][C:16](=[...
CCCCOC(=O)c1ccc(N)cc1.N#C[S-].O=C(Cl)c1ccc2ccccc2c1
CCCCOC(=O)c1ccc(NC(=S)NC(=O)c2ccc3ccccc3c2)cc1
null
null
CC(=O)C
Acylation
OtherReaction
ba32abf48e55d53ef6e0af57f1d7169ed0ac841ff7858c991011fd961a061dc2
b88d5f877c80e8bb46ad5808630e5b77d7f3aea35cbafadf6b92b5b8202ff7a7
O=C(NC(=S)Nc1ccccc1)c1ccc2ccccc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[N;H0;D1;+0:6]#[C;H0;D2;+0:7]-[S-;H0;D1:8].[NH2;D1;+0:9]-[c:10](:[c:11]):[c:12]>>[O;D1;H0:2]=[C;H0;D3;+0:1](-[NH;D2;+0:6]-[C;H0;D3;+0:7](=[S;H0;D1;+0:8])-[NH;D2;+0:9]-[c:10](:[c:11]):[c:12])-[c:3](:[c:4]):[c:5]
null
[]
null
null
1
HOUR
2-Naphthoyl chloride (190 mg, 1 mmol) is added to a solution of ammonium thiocyanate (200 mg, about 3 mmol) in acetone (5 ml) and stirred at room temperature for 1 hour. Butyl 4-aminobenzoate (180 mg, 0.93 mmol) is added to the reaction mixture. Stirring is continued overnight at room temperature. The solid, which form...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Nitrile.Primary amine
Thiourea.Secondary amide
null
null
c1ccccc1.c1ccc2ccccc2c1
Other
CC(=O)C
null
1
CCCCOC(=O)c1ccc(N)cc1.N#C[S-].O=C(Cl)c1ccc2ccccc2c1>CC(=O)C>CCCCOC(=O)c1ccc(NC(=S)NC(=O)c2ccc3ccccc3c2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3b497646d789449c819e60ce8634b53c
CCCCOC(=O)c1ccc(N=C=S)cc1.CNC(=O)COc1ccccc1>>CCCCOC(=O)c1ccc(NC(=S)N(C)C(=O)COc2ccccc2)cc1
CC(C)(C)[O-].[K+].O(C1=CC=CC=C1)CC(=O)NC.C(CCC)OC(C1=CC=C(C=C1)N=C=S)=O>>C(CCC)OC(C1=CC=C(C=C1)NC(=S)N(C(COC1=CC=CC=C1)=O)C)=O
[CH3:1][CH2:2][CH2:3][CH2:4][O:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([N:12]=[C:13]=[S:14])[cH:27][cH:28]1.[NH:15]([CH3:16])[C:17](=[O:18])[CH2:19][O:20][c:21]1[cH:22][cH:23][cH:24][cH:25][cH:26]1>>[CH3:1][CH2:2][CH2:3][CH2:4][O:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=[S:14])[N:15]([CH3:16])[C:17](=[O...
CCCCOC(=O)c1ccc(N=C=S)cc1.CNC(=O)COc1ccccc1
CCCCOC(=O)c1ccc(NC(=S)N(C)C(=O)COc2ccccc2)cc1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
5c3f709ce78dad45613b201efabf0dcb5ede491d0721b6f902048ff9fa018c70
43eda399ba8c48d07548472f2e4ea209c9863e42a9d42fa29ffa8a810d7a89a6
O=C(COc1ccccc1)NC(=S)Nc1ccccc1
[C:1]-[C:2](=[O;D1;H0:3])-[NH;D2;+0:4]-[C;D1;H3:5].[S;D1;H0:6]=[C;H0;D2;+0:7]=[N;H0;D2;+0:8]-[c:9](:[c:10]):[c:11]>>[C:1]-[C:2](=[O;D1;H0:3])-[N;H0;D3;+0:4](-[C;D1;H3:5])-[C;H0;D3;+0:7](=[S;D1;H0:6])-[NH;D2;+0:8]-[c:9](:[c:10]):[c:11]
10
[{"value": 10.0, "product": "C(CCC)OC(C1=CC=C(C=C1)NC(=S)N(C(COC1=CC=CC=C1)=O)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
t-BuOK (0.55 mL of 1.0 N solution) in THF is added to a solution of phenoxy-N-methylacetamide (83 mg, 0.5 mmol) in THF (5 mL). After 5 minutes, butyl-4-isothiocyanatobenzoate (118 mg, 0.5 mmol) is added in one portion and the resultant mixture is stirred overnight. The crude mixture is filtered through a silica pad. Af...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Isothiocyanate
Thiourea
null
null
c1ccccc1.c1ccccc1
null
C1CCOC1
null
0.083333
CCCCOC(=O)c1ccc(N=C=S)cc1.CNC(=O)COc1ccccc1>C1CCOC1>CCCCOC(=O)c1ccc(NC(=S)N(C)C(=O)COc2ccccc2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-32423f84d6c1444db24b353eaff2d0d9
C=Cc1ccccc1>>C=Cc1ccccc1
C=CC1=CC=CC=C1.C(C=C)#N.P(=O)([O-])([O-])[O-].[Ca+2].[Ca+2].[Ca+2].P(=O)([O-])([O-])[O-].CC(C)(C#N)N=NC(C)(C)C#N>>C=CC#N.C=CC1=CC=CC=C1
[CH2:5]=[CH:6][c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1>>[CH2:5]=[CH:6][c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1
C=Cc1ccccc1
C=Cc1ccccc1
null
null
O
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccccc1
null
null
[]
null
null
180
MINUTE
71 parts of styrene, 29 parts of acrylonitrile, 120 parts of deionized water and 0.2 parts of azobisisobutylonitrile (AIBN) were blended. To the blend, 0.5 parts of tricalciumphosphate and 0.3 parts of mercaptan-containing chain transfer agent were added. The resultant solution was heated to 80° C. for 90 minutes and k...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1
null
O
null
3
C=Cc1ccccc1>O>C=Cc1ccccc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2f21ab4ae6b24aae8d92c7c7db426ccc
O=C([O-])C1C2C=CC(C2)C1C(=O)[O-].[Na+]>>O=C([O-])C1C2CCC(C2)C1C(=O)[O-].[Na+]
C12C(C(C(C=C1)C2)C(=O)[O-])C(=O)[O-].[Na+].[Na+]>>C12C(C(C(CC1)C2)C(=O)[O-])C(=O)[O-].[Na+].[Na+]
[O:1]=[C:2]([O-:3])[CH:4]1[CH:5]2[CH:6]=[CH:7][CH:8]([CH2:9]2)[CH:10]1[C:11](=[O:12])[O-:13].[Na+:15]>>[O:1]=[C:2]([O-:3])[CH:4]1[CH:5]2[CH2:6][CH2:7][CH:8]([CH2:9]2)[CH:10]1[C:11](=[O:12])[O-:13].[Na+:15]
O=C([O-])C1C2C=CC(C2)C1C(=O)[O-].[Na+]
O=C([O-])C1C2CCC(C2)C1C(=O)[O-].[Na+]
null
[Pd]
O
Miscellaneous
OtherReaction
3f43743134a5de32528d95c060c25e5a7d7de42b355c50547d48d8cb02da2515
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
C1CC2CCC1C2
[O;-;D1;H0:1]-[C:2](=[O;D1;H0:3])-[C:4]1-[C:5](-[C:6](-[O;-;D1;H0:7])=[O;D1;H0:8])-[C:9]2-[C:10]-[C:11]-1-[CH;D2;+0:12]=[CH;D2;+0:13]-2>>[O;-;D1;H0:1]-[C:2](=[O;D1;H0:3])-[C:4]1-[C:5](-[C:6](-[O;-;D1;H0:7])=[O;D1;H0:8])-[C:9]2-[C:10]-[C:11]-1-[CH2;D2;+0:12]-[CH2;D2;+0:13]-2
null
[]
null
null
8
HOUR
To a solution of disodium bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate (10.0 g, from example 3) in water (100 g) was added 0.5 g palladium on activated carbon (5 wt %). The mixture was transferred into a Parr reactor and was subjected to hydrogenation (50 psi, room temperature) for 8 hours. The activated carbon was filte...
10.6084/m9.figshare.5104873.v1
null
null
null
C1=CC2CCC1C2
C1CC2CCC1C2
C1CC2CCC1C2
null
[Pd].O
null
8
O=C([O-])C1C2C=CC(C2)C1C(=O)[O-].[Na+]>[Pd].O>O=C([O-])C1C2CCC(C2)C1C(=O)[O-].[Na+]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c0156d75e2c14a898911d22916c87e2d
[Ca+2]>>[Ca+2]
C12C(C(C(CC1)C2)C(=O)[O-])C(=O)[O-].[Na+].[Na+].O.O.[Cl-].[Ca+2].[Cl-]>>C12C(C(C(CC1)C2)C(=O)[O-])C(=O)[O-].[Ca+2]
[Ca+2:14]>>[Ca+2:14]
[Ca+2]
[Ca+2]
null
null
O
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
60
CELSIUS
2
HOUR
To a solution of disodium bicyclo[2.2.1]heptane-2,3-dicarboxylate (22.6 g, 0.1 mol) in water (150 g) was added a solution of calcium chloride dihydrate (14.7 g, 0.1 mol) in water (100 g). The mixture stirred at 60° C. for 2 hours. The resulting white precipitate was filtered. The white powdery product was dried and mil...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
O
60
2
[Ca+2]>O>[Ca+2]
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9012a462bfb94024b4c6414b67674db0
C=CC(=O)OCCCC>>C=CC(=O)OCCCC
S(=O)(=O)(OCCCCCCCCCCCC)[O-].[Na+].C(C=C)#N.C(C=C)(=O)OCCCC>>C(C=C)#N.C(C=C)(=O)OCCCC
[CH2:5]=[CH:6][C:7](=[O:8])[O:9][CH2:10][CH2:11][CH2:12][CH3:13]>>[CH2:5]=[CH:6][C:7](=[O:8])[O:9][CH2:10][CH2:11][CH2:12][CH3:13]
C=CC(=O)OCCCC
C=CC(=O)OCCCC
null
null
O
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
80
CELSIUS
10
HOUR
Into a 2 L reactor equipped with an agitator, a thermometer, a nitrogen gas inlet tube, a dropping funnel, and a reflux condenser, was placed 600 g of distilled water, 0.71 g of sodium dodecyl sulfate as an emulsifier, and as monomers, 70 g of acrylonitrile and 30 g of n-butyl acrylate, and the reactor was nitrogen-pur...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
O
80
10
C=CC(=O)OCCCC>O>C=CC(=O)OCCCC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4a4ae9e8f6ba440f926878548739f414
C1CCCCC1.O=C(O)C1=CCCCC1>>O=C1C2=C(CCCC2)C2CCCCC12
C1(=CCCCC1)C(=O)O.C1CCCCC1.S(=O)(=O)([O-])[O-].[NH4+].[NH4+]>>C1CCCC2C=3CCCCC3C(C12)=O
[CH2:3]1[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]1.O[C:2](=[O:1])[C:14]1=[CH:9][CH2:10][CH2:11][CH2:12][CH2:13]1>>[O:1]=[C:2]1[C:3]2=[C:4]([CH2:5][CH2:6][CH2:7][CH2:8]2)[CH:9]2[CH2:10][CH2:11][CH2:12][CH2:13][CH:14]12
C1CCCCC1.O=C(O)C1=CCCCC1
O=C1C2=C(CCCC2)C2CCCCC12
null
null
O
C-C Coupling
OtherReaction
30b2100907c086f57836aa17450222e20e67139f5d22b81ca8cbd745fbb8324f
a49756d2995b35bf1c4b6840928f031562470ef5bd676447fb43ce2575147daa
O=C1C2=C(CCCC2)C2CCCCC12
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C;H0;D3;+0:3]1=[CH;D2;+0:4]-[C:5]-[C:6]-[C:7]-[C:8]-1.[C:9]1-[C:10]-[C:11]-[C:12]-[CH2;D2;+0:13]-[CH2;D2;+0:14]-1>>[O;D1;H0:2]=[C;H0;D3;+0:1]1-[C;H0;D3;+0:13]2=[C;H0;D3;+0:14](-[C:9]-[C:10]-[C:11]-[C:12]-2)-[CH;D3;+0:4]2-[C:5]-[C:6]-[C:7]-[C:8]-[CH;D3;+0:3]-1-2
43
[{"value": 43.0, "product": "C1CCCC2C=3CCCCC3C(C12)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
4.5
HOUR
In a 250 ml three neck round bottom flask, equipped with a mechanical stirrer, a thermometer and a reflux condenser 16.276 g of polyphosphoric acid was charged and heated to a temperature of 70° C. 16.276 g of 1-cyclohexenecarboxylic acid and 10.592 g of cyclohexane were added dropwise maintaining a temperature of the ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ketone
C1CCCCC1.C1=CCCCC1
C1CCC2=C(C1)CC1CCCCC21
C1CCC2=C(C1)CC1CCCCC21
HO-
O
70
4.5
C1CCCCC1.O=C(O)C1=CCCCC1>O>O=C1C2=C(CCCC2)C2CCCCC12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-079cc66065be4b169c9108c6a8bd6faf
O=C1C2=C(CCCC2)C2CCCCC12>>CC1=C2CCCCC2C2=C1CCCC2
Cl.C1CCCC2C=3CCCCC3C(C12)=O.C[Mg]Br>>CC=1C=2CCCCC2C2CCCCC12
O=[C:8]1[CH:3]2[CH:2]([CH2:7][CH2:6][CH2:5][CH2:4]2)[C:10]2=[C:9]1[CH2:14][CH2:13][CH2:12][CH2:11]2>>[CH3:1][C:2]1=[C:3]2[CH2:4][CH2:5][CH2:6][CH2:7][CH:8]2[C:9]2=[C:10]1[CH2:11][CH2:12][CH2:13][CH2:14]2
O=C1C2=C(CCCC2)C2CCCCC12
CC1=C2CCCCC2C2=C1CCCC2
null
null
O1CCCC1
Miscellaneous
OtherReaction
31a9ddf1be707eee87db5e81934c32eb6582706e14f7a8f4c3c9ec6e09b8e3ba
9db0f73aed071f5fa7238b261fc87a241efa69e871d2f239452605149d0c954e
C1=C2CCCCC2C2=C1CCCC2
O=[C;H0;D3;+0:1]1-[C:2](=[C:3](-[C:4])-[CH;D3;+0:5]2-[CH2;D2;+0:6]-[C:7]-[C:8]-[C:9]-[CH;D3;+0:10]-1-2)-[C:11]>>[C:4]-[C:3]1=[C:2](-[C:11])-[CH;D3;+0:1]2-[CH2;D2;+0:6]-[C:7]-[C:8]-[C:9]-[C;H0;D3;+0:10]-2=[C;H0;D3;+0:5]-1-[C;D1;H3:12]
92
[{"value": 92.0, "product": "CC=1C=2CCCCC2C2CCCCC12", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.8, "product": "CC=1C=2CCCCC2C2CCCCC12", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a solution of 1,2,3,4,4a,5,6,7,8,9a-decahydrofluoren-9-one (90.7 mg, 0.477 mmol) in tetrahydrofuran (5 ml), 0.35 ml (1.05 mmol) of methylmagnesium bromide (3.0 M in Et2O) was added dropwise under nitrogen at −78° C. The resulting cloudy mixture was kept at −78° C. for 3 hours and then allowed to warm to room tempera...
10.6084/m9.figshare.5104873.v1
null
Ketone
null
C1CCC2=C(C1)CC1CCCCC21
C1=C2CCCCC2C2=C1CCCC2
C1=C2CCCCC2C2=C1CCCC2
null
O1CCCC1
null
3
O=C1C2=C(CCCC2)C2CCCCC12>O1CCCC1>CC1=C2CCCCC2C2=C1CCCC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2089ca02cdbb49f195f3df439abb0e82
C1=CCCC1.O=C(O)C1=CCCC1>>O=C1C2=C(CCC2)[C@H]2CCC[C@@H]12
C1(=CCCC1)C(=O)O.C1=CCCC1>>C1=2C([C@@H]3CCC[C@@H]3C2CCC1)=O
[CH:8]1=[CH:12][CH2:11][CH2:10][CH2:9]1.O=[C:2]([OH:1])[C:3]1=[CH:4][CH2:5][CH2:6][CH2:7]1>>[O:1]=[C:2]1[C:3]2=[C:4]([CH2:5][CH2:6][CH2:7]2)[C@H:8]2[CH2:9][CH2:10][CH2:11][C@@H:12]12
C1=CCCC1.O=C(O)C1=CCCC1
O=C1C2=C(CCC2)[C@H]2CCC[C@@H]12
null
null
S(=O)(=O)([O-])[O-].[NH4+].[NH4+]
Acylation
OtherReaction
2fce04924b3f49945a37977f6822da19258f5fda09c938ebedc90ef567e3eb62
26fa8fd71cdd2db70d55c60f92a5587664090781bde28495d3bab102e1ae668a
O=C1C2=C(CCC2)[C@H]2CCC[C@@H]12
O=[C;H0;D3;+0:1](-[OH;D1;+0:2])-[C:3]1=[CH;D2;+0:4]-[C:5]-[C:6]-[C:7]-1.[C:8]1-[C:9]-[CH;D2;+0:10]=[CH;D2;+0:11]-[C:12]-1>>[O;H0;D1;+0:2]=[C;H0;D3;+0:1]1-[C:3]2=[C;H0;D3;+0:4](-[C:5]-[C:6]-[C:7]-2)-[C@H;D3;+0:11]2-[C:12]-[C:8]-[C:9]-[C@@H;D3;+0:10]-1-2
null
[]
30
CELSIUS
4
HOUR
A stirred suspension of 1-cyclopentene carboxylic acid (11.2 g, 100 mmol) and cyclopentene (13.6 g, 200 mmol) was added slowly to stirring polyphosphoric acid (Aldrich, 300 g) at 60° C. in a 250 mL flask. The reaction mixture was stirred at 70–80° C. for 4 hours under nitrogen. The dark brown reaction mixture was coole...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ketone
C1=CCCC1.C1=CCCC1
C1CC2=C(C1)[C@H]1CCC[C@H]1C2
C1CC2=C(C1)[C@H]1CCC[C@H]1C2
HO-
S(=O)(=O)([O-])[O-].[NH4+].[NH4+]
30
4
C1=CCCC1.O=C(O)C1=CCCC1>S(=O)(=O)([O-])[O-].[NH4+].[NH4+]>O=C1C2=C(CCC2)[C@H]2CCC[C@@H]12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e7e86c6093174ea1bac2f28462d3f752
CC(C)(C)OC(=O)NCCCN.O=S(=O)(Cl)c1cccc2cnccc12>>CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCN.C(C)N(CC)CC.C1=NC=CC=2C(=CC=CC12)S(=O)(=O)Cl>>C(C)(C)(C)OC(=O)NCCCNS(=O)(=O)C1=C2C=CN=CC2=CC=C1
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][NH2:12].Cl[S:13](=[O:14])(=[O:15])[c:16]1[cH:17][cH:18][cH:19][c:20]2[cH:21][n:22][cH:23][cH:24][c:25]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][NH:12][S:13](=[O:14])(=[O:15])[c:16]1[cH:17][cH:18][cH:19]...
CC(C)(C)OC(=O)NCCCN.O=S(=O)(Cl)c1cccc2cnccc12
CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2cnccc12
null
null
ClCCl
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
c1ccc2cnccc2c1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
null
[]
null
null
30
MINUTE
A solution of N-(tert-butoxycarbonyl)-1,3-propylenediamine (2.09 g, Tokyo Kasei Kogyo) and triethylamine (3.4 ml, Tokyo Kasei Kogyo) in dichloromethane (20 ml) was added with a solution of isoquinoline-5-sulfonyl chloride (2.73 g, prepared according to Japanese Patent Unexamined Publication (Kokai) No. 61-227581) in di...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2cnccc2c1
HCl
ClCCl
null
0.5
CC(C)(C)OC(=O)NCCCN.O=S(=O)(Cl)c1cccc2cnccc12>ClCCl>CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-99be45a0fb164c68b4577c67d8e9e37e
CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2cnccc12.CCCCP(CCCC)CCCC.CN(C)C(=O)N=NC(=O)N(C)C>>CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCNS(=O)(=O)C1=C2C=CN=CC2=CC=C1.N(=NC(=O)N(C)C)C(=O)N(C)C.C1(=CC=CC=C1)CCCO.C(CCC)P(CCCC)CCCC>>C(C)(C)(C)OC(=O)NCCCN(CCCC1=CC=CC=C1)S(=O)(=O)C1=C2C=CN=CC2=CC=C1.C1(=CC=CC=C1)CCCO
[CH3:1][C:2]([CH3:4])([O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][NH:12][S:22](=[O:23])(=[O:24])[c:25]1[cH:26][cH:27][cH:28][c:29]2[cH:30][n:31][cH:32][cH:33][c:34]12)[CH3:17].CC[CH2:14][CH2:15]P(CCC[CH3:18])[CH2:19][CH2:20][CH2:21][CH3:16].CN(C)C(=O)N=NC(=O)N([CH3:3])[CH3:13]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C...
CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2cnccc12.CCCCP(CCCC)CCCC.CN(C)C(=O)N=NC(=O)N(C)C
CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
null
null
O1CCCC1
Aromatic Heterocycle Formation
OtherReaction
8337f786eb5fde5cab8e70a191935fd4582a55c6eff8a0b3bf08e5877685842e
51b0ac63f70b1c36d791c24a3cb1506a541098df476fbc0f63b74e39d5ee1859
O=S(=O)(NCCCc1ccccc1)c1cccc2cnccc12
C-C-[CH2;D2;+0:1]-[CH2;D2;+0:2]-P(-C-C-C-[CH3;D1;+0:3])-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[CH3;D1;+0:7].C-N(-C)-C(=O)-N=N-C(=O)-N(-[CH3;D1;+0:8])-[CH3;D1;+0:9].[#7:10]-[C:11](=[O;D1;H0:12])-[#8:13]-[C;H0;D4;+0:14](-[C;D1;H3:15])(-[C;D1;H3:16])-[CH3;D1;+0:17].[C:18]-[C:19]-[NH;D2;+0:20]-[#16:21](=[O;D1;H0:22])(=...
null
[]
null
null
null
null
A solution of Intermediate 1 (640 mg), 1,1′-azobis(N,N-dimethylformamide) (1200 mg, Aldrich or prepared according to Chemistry Letters, 539 (1994)) and 3-phenyl-1-propanol (710 μl, Tokyo Kasei Kogyo) in tetrahydrofuran (30 ml) was added with tri(n-butyl)phosphine (1.75 ml, Tokyo Kasei Kogyo) with stirring and ice cooli...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Ether.Diazene.Tertiary amide.Tertiary amide.Boc
Ether.Tertiary amine.Boc
null
c1ccccc1
c1ccccc1.c1ccc2cnccc2c1
HO-
O1CCCC1
null
null
CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2cnccc12.CCCCP(CCCC)CCCC.CN(C)C(=O)N=NC(=O)N(C)C>O1CCCC1>CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-62100151a08f44888e9b9f008aa8d719
CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12>>NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCN(CCCC1=CC=CC=C1)S(=O)(=O)C1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCCN)CCCC1=CC=CC=C1
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][CH2:9][c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)[S:16](=[O:17])(=[O:18])[c:19]1[cH:20][cH:21][cH:22][c:23]2[cH:24][n:25][cH:26][cH:27][c:28]12>>[NH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][CH2:9][c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)[S:16](=[O:17...
CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(NCCCc1ccccc1)c1cccc2cnccc12
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
25
MINUTE
Intermediate 2 (913 mg) was added with 10% hydrogen chloride/methanol solution (18 ml, Tokyo Kasei Kogyo) at room temperature and stirred for 25 minutes under reflux by heating. After the reaction, the solvent was evaporated under reduced pressure, and the residue was crystallized from a mixed solvent of methanol and d...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
null
null
0.416667
CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12>>NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b5e351201461494c8b84873e8fe9cd2a
CC(C)(C)OC(=O)NCCCN(CCc1cccs1)S(=O)(=O)c1cccc2cnccc12>>NCCCN(CCc1cccs1)S(=O)(=O)c1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCN(CCC=1SC=CC1)S(=O)(=O)C1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCCN)CCC=1SC=CC1
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][s:13]1)[S:14](=[O:15])(=[O:16])[c:17]1[cH:18][cH:19][cH:20][c:21]2[cH:22][n:23][cH:24][cH:25][c:26]12>>[NH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][c:9]1[cH:10][cH:11][cH:12][s:13]1)[S:14](=[O:15])(=[O:16])[c:17]1[cH:18][cH:19]...
CC(C)(C)OC(=O)NCCCN(CCc1cccs1)S(=O)(=O)c1cccc2cnccc12
NCCCN(CCc1cccs1)S(=O)(=O)c1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(NCCc1cccs1)c1cccc2cnccc12
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
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 3 (238 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with meth...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccsc1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCCN(CCc1cccs1)S(=O)(=O)c1cccc2cnccc12>>NCCCN(CCc1cccs1)S(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-40e9753b7e624fac9a959e0125d91815
CC(C)(C)OC(=O)NCCCN(CCCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12>>NCCCN(CCCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCN(CCCCC1=CC=CC=C1)S(=O)(=O)C1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCCN)CCCCC1=CC=CC=C1
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][CH2:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[S:17](=[O:18])(=[O:19])[c:20]1[cH:21][cH:22][cH:23][c:24]2[cH:25][n:26][cH:27][cH:28][c:29]12>>[NH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][CH2:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16...
CC(C)(C)OC(=O)NCCCN(CCCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
NCCCN(CCCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(NCCCCc1ccccc1)c1cccc2cnccc12
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
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 6 (249 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with meth...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCCN(CCCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12>>NCCCN(CCCCc1ccccc1)S(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a776e1ae388e4dcfab81dc757e40f082
Cc1cncc2cccc(S(=O)(=O)N(CCCNC(=O)OC(C)(C)C)CCCc3ccccc3)c12>>Cc1cncc2cccc(S(=O)(=O)N(CCCN)CCCc3ccccc3)c12
C(C)(C)(C)OC(=O)NCCCN(CCCC1=CC=CC=C1)S(=O)(=O)C1=C2C(=CN=CC2=CC=C1)C.Cl.CO>>Cl.CC1=CN=CC2=CC=CC(=C12)S(=O)(=O)N(CCCN)CCCC1=CC=CC=C1
CC(C)(C)OC(=O)[NH:18][CH2:17][CH2:16][CH2:15][N:14]([S:11]([c:10]1[cH:9][cH:8][cH:7][c:6]2[cH:5][n:4][cH:3][c:2]([CH3:1])[c:28]21)(=[O:12])=[O:13])[CH2:19][CH2:20][CH2:21][c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([S:11](=[O:12])(=[O:13])[N:14]([CH2:15][CH2...
Cc1cncc2cccc(S(=O)(=O)N(CCCNC(=O)OC(C)(C)C)CCCc3ccccc3)c12
Cc1cncc2cccc(S(=O)(=O)N(CCCN)CCCc3ccccc3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(NCCCc1ccccc1)c1cccc2cnccc12
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
null
null
According to the method of Example 1, Step C, deprotection was performed (5° C., 2 hours) by using Intermediate 8 (87 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and the solvent was evaporated under reduced pressure. The residue was added with methanol (1...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.c1ccccc1
HO-
null
null
null
Cc1cncc2cccc(S(=O)(=O)N(CCCNC(=O)OC(C)(C)C)CCCc3ccccc3)c12>>Cc1cncc2cccc(S(=O)(=O)N(CCCN)CCCc3ccccc3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-157b347806e5402d819b7c9214a3f0d4
CC(C)(C)OC(=O)NCCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12>>NCCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCN(CCS(=O)(=O)C1=CC=CC=C1)S(=O)(=O)C1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCCN)CCS(=O)(=O)C1=CC=CC=C1
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][S:9](=[O:10])(=[O:11])[c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1)[S:18](=[O:19])(=[O:20])[c:21]1[cH:22][cH:23][cH:24][c:25]2[cH:26][n:27][cH:28][cH:29][c:30]12>>[NH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][S:9](=[O:10])(=[O:11])[c:12]1[cH:13][cH:14][cH:...
CC(C)(C)OC(=O)NCCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12
NCCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(CCNS(=O)(=O)c1cccc2cnccc12)c1ccccc1
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
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 9 (266 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with meth...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12>>NCCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-87611e49e57f41e0aa291dec7a4e4ee9
CC(C)(C)OC(=O)NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12>>NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCN(CCS(=O)(=O)C1=CC=CC=C1)S(=O)(=O)C1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCN)CCS(=O)(=O)C1=CC=CC=C1
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][N:5]([CH2:6][CH2:7][S:8](=[O:9])(=[O:10])[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[S:17](=[O:18])(=[O:19])[c:20]1[cH:21][cH:22][cH:23][c:24]2[cH:25][n:26][cH:27][cH:28][c:29]12>>[NH2:2][CH2:3][CH2:4][N:5]([CH2:6][CH2:7][S:8](=[O:9])(=[O:10])[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16...
CC(C)(C)OC(=O)NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12
NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(CCNS(=O)(=O)c1cccc2cnccc12)c1ccccc1
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
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 11 (260 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12>>NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0b98f7d580184ebbb6b7dbce359be919
CC(C)(C)OC(=O)NCCCN.O=S(=O)(Cl)c1cccc2c(Cl)nccc12>>CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2c(Cl)nccc12
Cl.ClC1=NC=CC2=C(C=CC=C12)S(=O)(=O)Cl.C(C)(C)(C)OC(NCCCN)=O.C(C)N(CC)CC.ClC1=NC=CC2=C(C=CC=C12)S(=O)(=O)Cl>>C(C)(C)(C)OC(=O)NCCCNS(=O)(=O)C1=C2C=CN=C(C2=CC=C1)Cl
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][NH2:12].Cl[S:13](=[O:14])(=[O:15])[c:16]1[cH:17][cH:18][cH:19][c:20]2[c:21]([Cl:22])[n:23][cH:24][cH:25][c:26]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][NH:12][S:13](=[O:14])(=[O:15])[c:16]1[cH:17][cH:18...
CC(C)(C)OC(=O)NCCCN.O=S(=O)(Cl)c1cccc2c(Cl)nccc12
CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2c(Cl)nccc12
null
null
ClCCl
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
c1ccc2cnccc2c1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]
null
[]
null
null
20
HOUR
According to the method of Example 1, Step A, a solution of N-(3-aminopropyl)carbamic acid tert-butyl ester (383 mg) and triethylamine (335 μl) in dichloromethane (3 ml) was added with a solution of (1-chloro-5-isoquinolyl)sulfonyl chloride (524 mg, prepared from (1-chloro-5-isoquinolyl)sulfonyl chloride hydrochloride ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccc2cnccc2c1
HCl
ClCCl
null
20
CC(C)(C)OC(=O)NCCCN.O=S(=O)(Cl)c1cccc2c(Cl)nccc12>ClCCl>CC(C)(C)OC(=O)NCCCNS(=O)(=O)c1cccc2c(Cl)nccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1f0fc8e12b234911a16444002c85ac20
CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12>>NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12
NC1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCCNC(=O)OC(C)(C)C)CCCC1=CC=CC=C1.Cl.CO>>Cl.NC1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCCN)CCCC1=CC=CC=C1
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][CH2:9][c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)[S:16](=[O:17])(=[O:18])[c:19]1[cH:20][cH:21][cH:22][c:23]2[c:24]([NH2:25])[n:26][cH:27][cH:28][c:29]12>>[NH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:7][CH2:8][CH2:9][c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)[S:1...
CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12
NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(NCCCc1ccccc1)c1cccc2cnccc12
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
null
null
According to the method of Example 1, Step C, deprotection was performed (5° C., 2 hours) by using Intermediate 14 (125 mg) and 10% hydrogen chloride/methanol solution (2.5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12>>NCCCN(CCCc1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cfd70b3b3b30460cbdf9d354bc36adca
CC(C)(C)OC(=O)NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12>>NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12
NC1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCNC(=O)OC(C)(C)C)CCS(=O)(=O)C1=CC=CC=C1.Cl.CO>>Cl.NC1=NC=CC2=C(C=CC=C12)S(=O)(=O)N(CCN)CCS(=O)(=O)C1=CC=CC=C1
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][N:5]([CH2:6][CH2:7][S:8](=[O:9])(=[O:10])[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[S:17](=[O:18])(=[O:19])[c:20]1[cH:21][cH:22][cH:23][c:24]2[c:25]([NH2:26])[n:27][cH:28][cH:29][c:30]12>>[NH2:2][CH2:3][CH2:4][N:5]([CH2:6][CH2:7][S:8](=[O:9])(=[O:10])[c:11]1[cH:12][cH:13][cH:14][cH:...
CC(C)(C)OC(=O)NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12
NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12
null
null
C(C)OCC
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=S(=O)(CCNS(=O)(=O)c1cccc2cnccc12)c1ccccc1
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
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 17 (134 mg) and 10% hydrogen chloride/methanol solution (2.5 ml). The reaction mixture was cooled to room temperature and then added with diethyl ether (2.5 ml). The deposited precipitates were collected by ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
C(C)OCC
null
null
CC(C)(C)OC(=O)NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12>C(C)OCC>NCCN(CCS(=O)(=O)c1ccccc1)S(=O)(=O)c1cccc2c(N)nccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-881ac3f56ed04e33b46fda327ae9d93f
CC(C)(C)OC(=O)NCCCO.Oc1cccc2c(Cl)nccc12>>CC(C)(C)OC(=O)NCCCOc1cccc2c(Cl)nccc12
C(CCC)P(CCCC)CCCC.ClC1=NC=CC2=C(C=CC=C12)O.C(C)(C)(C)OC(NCCCO)=O.N(=NC(=O)N(C)C)C(=O)N(C)C>>C(C)(C)(C)OC(=O)NCCCOC1=C2C=CN=C(C2=CC=C1)Cl
O[CH2:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7].[OH:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[c:18]([Cl:19])[n:20][cH:21][cH:22][c:23]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][O:12][c:13]1[cH:14][cH:15][cH:16][c:17]2[c:18]([Cl:19])[n:20][cH:21][cH:22][...
CC(C)(C)OC(=O)NCCCO.Oc1cccc2c(Cl)nccc12
CC(C)(C)OC(=O)NCCCOc1cccc2c(Cl)nccc12
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether
86bfb73617450d22f9456ed5ce4d96a73f1f8fc0c016bebae57fda68e2da86a2
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccc2cnccc2c1
O-[CH2;D2;+0:1]-[C:2]-[C:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
null
[]
null
null
24
HOUR
A suspension of 1-chloro-5-hydroxyisoquinoline (539 mg, synthesized according to the method described in a reference (Georgian, V. et al., J. Org. Chem., 27, 4571 (1962))), (3-hydroxypropyl)carbamic acid tert-butyl ester (1.58 g, Tokyo Kasei Kogyo) and 1,1′-azobis(N,N-dimethylformamide) (1.55 g) in tetrahydrofuran (8 m...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
null
c1ccc2cnccc2c1
HO-
O1CCCC1
null
24
CC(C)(C)OC(=O)NCCCO.Oc1cccc2c(Cl)nccc12>O1CCCC1>CC(C)(C)OC(=O)NCCCOc1cccc2c(Cl)nccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2e01521f8a6a49748b5268aa0846e201
CC(C)(C)OC(=O)NCCCOc1cccc2c(Cl)nccc12>>Cl.NCCCOc1cccc2c(N)nccc12
C(C)(C)(C)OC(=O)NCCCOC1=C2C=CN=C(C2=CC=C1)Cl.C(C)(C)(C)OC(=O)NCCCOC1=C2C=CN=C(C2=CC=C1)Cl.C(C)(C)(C)P(C1=C(C=CC=C1)C1=CC=CC=C1)C(C)(C)C.COC1=CC=C(CN)C=C1.CC(C)([O-])C.[Na+]>>Cl.NC1=NC=CC2=C(C=CC=C12)OCCCN
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][O:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([Cl:1])[n:14][cH:15][cH:16][c:17]12>>[ClH:1].[NH2:2][CH2:3][CH2:4][CH2:5][O:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([NH2:13])[n:14][cH:15][cH:16][c:17]12
CC(C)(C)OC(=O)NCCCOc1cccc2c(Cl)nccc12
Cl.NCCCOc1cccc2c(N)nccc12
null
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd]
C(C)(=O)OCC.C1(=CC=CC=C1)C
Miscellaneous
OtherReaction
ca47f18fdd8a333ba739357322d7eea24bf7b08489a81c071de05fff408e8608
08bb0e341d3145616cc2674a463d3dbf2fc29e30c174b6945e30ce804e6809c3
c1ccc2cnccc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3].[Cl;H0;D1;+0:4]-[c;H0;D3;+0:5](:[#7;a:6]:[c:7]):[c:8](:[c:9]):[c:10]>>[C:3]-[C:2]-[NH2;D1;+0:1].[N;D1;H2:11]-[c;H0;D3;+0:5](:[#7;a:6]:[c:7]):[c:8](:[c:9]):[c:10].[ClH;D0;+0:4]
null
[]
80
CELSIUS
null
null
The title compound was synthesized from Intermediate 18 according to the method described in a reference (Buchwald, S. L., J. Org. Chem., 65, 1158 (2000)). That is, a suspension of Intermediate 18 (674 mg), tris (dibenzylideneacetone)dipalladium(0) (92 mg, Aldrich), 2-(di-tert-butylphosphino)biphenyl (119 mg, Strem Che...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ether.Boc
Primary amine.Primary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HO-
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C(C)(=O)OCC.C1(=CC=CC=C1)C
80
null
CC(C)(C)OC(=O)NCCCOc1cccc2c(Cl)nccc12>C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C(C)(=O)OCC.C1(=CC=CC=C1)C>Cl.NCCCOc1cccc2c(N)nccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-40b53d9bfdf444818e70852330749f6c
CC(C)(C)OC(=O)NCCCOc1cccc2c(N)nccc12>>NCCCOc1cccc2c(N)nccc12
C(C)(C)(C)OC(=O)NCCCOC1=C2C=CN=C(C2=CC=C1)N.Cl.CO>>Cl.NC1=NC=CC2=C(C=CC=C12)OCCCN
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][O:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([NH2:13])[n:14][cH:15][cH:16][c:17]12>>[NH2:2][CH2:3][CH2:4][CH2:5][O:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[c:12]([NH2:13])[n:14][cH:15][cH:16][c:17]12
CC(C)(C)OC(=O)NCCCOc1cccc2c(N)nccc12
NCCCOc1cccc2c(N)nccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2cnccc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 20 (159 mg) and 10% hydrogen chloride/methanol solution (2.5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with m...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCCOc1cccc2c(N)nccc12>>NCCCOc1cccc2c(N)nccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-31ed84e073364a278a09080c0b0a2456
CC(C)(C)OC(=O)N1CCCC(COc2cccc3c(N)nccc23)C1>>Nc1nccc2c(OCC3CCCNC3)cccc12
C(C)(C)(C)OC(=O)N1CC(CCC1)COC1=C2C=CN=C(C2=CC=C1)N.Cl.CO>>Cl.NC1=NC=CC2=C(C=CC=C12)OCC1CNCCC1
CC(C)(C)OC(=O)[N:15]1[CH2:14][CH2:13][CH2:12][CH:11]([CH2:10][O:9][c:8]2[c:7]3[cH:6][cH:5][n:4][c:3]([NH2:2])[c:20]3[cH:19][cH:18][cH:17]2)[CH2:16]1>>[NH2:2][c:3]1[n:4][cH:5][cH:6][c:7]2[c:8]([O:9][CH2:10][CH:11]3[CH2:12][CH2:13][CH2:14][NH:15][CH2:16]3)[cH:17][cH:18][cH:19][c:20]12
CC(C)(C)OC(=O)N1CCCC(COc2cccc3c(N)nccc23)C1
Nc1nccc2c(OCC3CCCNC3)cccc12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(OCC2CCCNC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:5]-[C:4]-[NH;D2;+0:1]-[C:2]-[C:3]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 23 (179 mg) and 10% hydrogen chloride/methanol solution (2.5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with m...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCCC(COc2cccc3c(N)nccc23)C1>>Nc1nccc2c(OCC3CCCNC3)cccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-236c7339795b45e393f5e303add9f945
Brc1cccc2cnccc12.CC(C)(C)OC(=O)NCCN>>CC(C)(C)OC(=O)NCCNc1cccc2cnccc12
BrC1=C2C=CN=CC2=CC=C1.C(C)(C)(C)P(C1=C(C=CC=C1)C1=CC=CC=C1)C(C)(C)C.C(C)(C)(C)OC(NCCN)=O.CC(C)([O-])C.[Na+]>>C(C)(C)(C)OC(=O)NCCNC1=C2C=CN=CC2=CC=C1
Br[c:12]1[cH:13][cH:14][cH:15][c:16]2[cH:17][n:18][cH:19][cH:20][c:21]12.[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][NH2:11]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][NH:11][c:12]1[cH:13][cH:14][cH:15][c:16]2[cH:17][n:18][cH:19][cH:20][c:21]12
Brc1cccc2cnccc12.CC(C)(C)OC(=O)NCCN
CC(C)(C)OC(=O)NCCNc1cccc2cnccc12
null
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd]
C(C)(=O)OCC.C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
17c3dbb58f19c559a89452c2c52a32d81319b5dd6d11e225611cc478eba61c1b
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2cnccc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[C:10]-[C:11]-[NH2;D1;+0:12]>>[C:10]-[C:11]-[NH;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
70
[{"value": 70.0, "product": "C(C)(C)(C)OC(=O)NCCNC1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
Under nitrogen atmosphere, a suspension of 5-bromoisoquinoline (416 mg, Spex), tris(dibenzylideneacetone)dipalladium(0) (92 mg), 2-(di-tert-butylphosphino)biphenyl (119 mg), N-(2-aminoethyl)carbamic acid tert-butyl ester (385 mg) and sodium tert-butoxide (269 mg) in toluene (5 ml) was stirred with heating at 80° C. for...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HBr
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C(C)(=O)OCC.C1(=CC=CC=C1)C
80
null
Brc1cccc2cnccc12.CC(C)(C)OC(=O)NCCN>C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C(C)(=O)OCC.C1(=CC=CC=C1)C>CC(C)(C)OC(=O)NCCNc1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-83ccd6a730cf4a3f904464d1133a0cd4
CC(C)(C)OC(=O)NCCNc1cccc2cnccc12>>NCCNc1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCNC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NCCN
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][NH:5][c:6]1[cH:7][cH:8][cH:9][c:10]2[cH:11][n:12][cH:13][cH:14][c:15]12>>[NH2:2][CH2:3][CH2:4][NH:5][c:6]1[cH:7][cH:8][cH:9][c:10]2[cH:11][n:12][cH:13][cH:14][c:15]12
CC(C)(C)OC(=O)NCCNc1cccc2cnccc12
NCCNc1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2cnccc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 27 (287 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCNc1cccc2cnccc12>>NCCNc1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5d0c38bbf7054bdc8ce5961cd8721103
CC(C)(C)OC(=O)NCCCNc1cccc2cnccc12>>NCCCNc1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCNC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NCCCN
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[cH:12][n:13][cH:14][cH:15][c:16]12>>[NH2:2][CH2:3][CH2:4][CH2:5][NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[cH:12][n:13][cH:14][cH:15][c:16]12
CC(C)(C)OC(=O)NCCCNc1cccc2cnccc12
NCCCNc1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2cnccc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 28 (301 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCCNc1cccc2cnccc12>>NCCCNc1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-34859159c1f24492b072bc7bfbc36a45
Brc1cccc2cnccc12.CN(CCCN)C(=O)OC(C)(C)C>>CN(CCCNc1cccc2cnccc12)C(=O)OC(C)(C)C
BrC1=C2C=CN=CC2=CC=C1.C(C)(C)(C)P(C1=C(C=CC=C1)C1=CC=CC=C1)C(C)(C)C.C(C)(C)(C)OC(N(C)CCCN)=O.CC(C)([O-])C.[Na+]>>C(C)(C)(C)OC(=O)N(CCCNC1=C2C=CN=CC2=CC=C1)C
Br[c:7]1[cH:8][cH:9][cH:10][c:11]2[cH:12][n:13][cH:14][cH:15][c:16]12.[CH3:1][N:2]([CH2:3][CH2:4][CH2:5][NH2:6])[C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23]>>[CH3:1][N:2]([CH2:3][CH2:4][CH2:5][NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[cH:12][n:13][cH:14][cH:15][c:16]12)[C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:...
Brc1cccc2cnccc12.CN(CCCN)C(=O)OC(C)(C)C
CN(CCCNc1cccc2cnccc12)C(=O)OC(C)(C)C
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
17c3dbb58f19c559a89452c2c52a32d81319b5dd6d11e225611cc478eba61c1b
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2cnccc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[C:10]-[C:11]-[NH2;D1;+0:12]>>[C:10]-[C:11]-[NH;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
85.1
[{"value": 85.1, "product": "C(C)(C)(C)OC(=O)N(CCCNC1=C2C=CN=CC2=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
null
null
Under nitrogen atmosphere, a suspension of 5-bromoisoquinoline (252 mg), tris(dibenzylideneacetone)palladium(0) (59 mg), 2-(di-tert-butylphosphino)biphenyl (74 mg), (3-aminopropyl)methylcarbamic acid tert-butyl ester (274 mg, Asta Tech), and sodium tert-butoxide (163 mg) in toluene was stirred with heating at 70° C. fo...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HBr
C1(=CC=CC=C1)C
70
null
Brc1cccc2cnccc12.CN(CCCN)C(=O)OC(C)(C)C>C1(=CC=CC=C1)C>CN(CCCNc1cccc2cnccc12)C(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e9e223d3e3e74eb7b824227dc02c0a1d
CN(CCCNc1cccc2cnccc12)C(=O)OC(C)(C)C>>CNCCCNc1cccc2cnccc12
C(C)(C)(C)OC(=O)N(CCCNC1=C2C=CN=CC2=CC=C1)C.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NCCCNC
CC(C)(C)OC(=O)[N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[cH:12][n:13][cH:14][cH:15][c:16]12>>[CH3:1][NH:2][CH2:3][CH2:4][CH2:5][NH:6][c:7]1[cH:8][cH:9][cH:10][c:11]2[cH:12][n:13][cH:14][cH:15][c:16]12
CN(CCCNc1cccc2cnccc12)C(=O)OC(C)(C)C
CNCCCNc1cccc2cnccc12
null
null
null
Reduction
Boc amine deprotection
bbda4640db5f48af4538caded12fdadd56eacd6d4e5f7aefe46282d665df167e
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc2cnccc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C;D1;H3:2])-[C:3]-[C:4]>>[C:4]-[C:3]-[NH;D2;+0:1]-[C;D1;H3:2]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 31 hours) by using Intermediate 29 (325 mg) and 10% hydrogen chloride/methanol solution (5 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (1 ml) and diethyl ether (3 ml). The depo...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
null
null
c1ccc2cnccc2c1
HO-
null
null
null
CN(CCCNc1cccc2cnccc12)C(=O)OC(C)(C)C>>CNCCCNc1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-672a2fed6b53437e84c0e43685bb65b1
CC(C)(C)OC(=O)NCCCCNc1cccc2cnccc12>>NCCCCNc1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCCNC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NCCCCN
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][CH2:6][NH:7][c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][n:14][cH:15][cH:16][c:17]12>>[NH2:2][CH2:3][CH2:4][CH2:5][CH2:6][NH:7][c:8]1[cH:9][cH:10][cH:11][c:12]2[cH:13][n:14][cH:15][cH:16][c:17]12
CC(C)(C)OC(=O)NCCCCNc1cccc2cnccc12
NCCCCNc1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2cnccc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 30 (316 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCCCNc1cccc2cnccc12>>NCCCCNc1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-600f4b91275841b0837efb247cf9997c
Brc1cccc2cnccc12.CC(C)(C)OC(=O)NCCCCCN>>CC(C)(C)OC(=O)NCCCCCNc1cccc2cnccc12
BrC1=C2C=CN=CC2=CC=C1.C(C)(C)(C)P(C1=C(C=CC=C1)C1=CC=CC=C1)C(C)(C)C.C(C)(C)(C)OC(NCCCCCN)=O.CC(C)([O-])C.[Na+]>>C(C)(C)(C)OC(=O)NCCCCCNC1=C2C=CN=CC2=CC=C1
Br[c:15]1[cH:16][cH:17][cH:18][c:19]2[cH:20][n:21][cH:22][cH:23][c:24]12.[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][NH2:14]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][NH:14][c:15]1[cH:16][cH:17][cH:18][c:19]2[cH:20][n...
Brc1cccc2cnccc12.CC(C)(C)OC(=O)NCCCCCN
CC(C)(C)OC(=O)NCCCCCNc1cccc2cnccc12
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
17c3dbb58f19c559a89452c2c52a32d81319b5dd6d11e225611cc478eba61c1b
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc2cnccc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[C:10]-[C:11]-[NH2;D1;+0:12]>>[C:10]-[C:11]-[NH;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1
84.3
[{"value": 84.3, "product": "C(C)(C)(C)OC(=O)NCCCCCNC1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
null
null
Under nitrogen atmosphere, a suspension of 5-bromoisoquinoline (245 mg), tris(dibenzylideneacetone)palladium(0) (56 mg), 2-(di-tert-butylphosphino)biphenyl (69 mg), N-(5-aminopentyl)carbamic acid tert-butyl ester (282 mg, Tokyo Kasei Kogyo) and sodium tert-butoxide (160 mg) in toluene was stirred with heating at 70° C....
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
c1ccc2cnccc2c1
HBr
C1(=CC=CC=C1)C
70
null
Brc1cccc2cnccc12.CC(C)(C)OC(=O)NCCCCCN>C1(=CC=CC=C1)C>CC(C)(C)OC(=O)NCCCCCNc1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-95aa8b8184824c4f92502d147d13a2fb
CC(C)(C)OC(=O)NCCCCCNc1cccc2cnccc12>>NCCCCCNc1cccc2cnccc12
C(C)(C)(C)OC(=O)NCCCCCNC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NCCCCCN
CC(C)(C)OC(=O)[NH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH:8][c:9]1[cH:10][cH:11][cH:12][c:13]2[cH:14][n:15][cH:16][cH:17][c:18]12>>[NH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH:8][c:9]1[cH:10][cH:11][cH:12][c:13]2[cH:14][n:15][cH:16][cH:17][c:18]12
CC(C)(C)OC(=O)NCCCCCNc1cccc2cnccc12
NCCCCCNc1cccc2cnccc12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc2cnccc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
null
null
null
null
According to the method of the above Example, deprotection was performed (room temperature, 31 hours) by using Intermediate 31 (327 mg) and 10% hydrogen chloride/methanol solution (5 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (1 ml) and diethyl ether (3 ml). The depo...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCCCCCNc1cccc2cnccc12>>NCCCCCNc1cccc2cnccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6faf4ab15932459f9790d3c18a3b64cc
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cnccc23)CC1>>c1cc(NC2CCNCC2)c2ccncc2c1
C1=NC=CC2=C(C=CC=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:9]1[CH2:8][CH2:7][CH:6]([NH:5][c:4]2[cH:3][cH:2][cH:18][c:17]3[c:12]2[cH:13][cH:14][n:15][cH:16]3)[CH2:11][CH2:10]1>>[cH:2]1[cH:3][c:4]([NH:5][CH:6]2[CH2:7][CH2:8][NH:9][CH2:10][CH2:11]2)[c:12]2[cH:13][cH:14][n:15][cH:16][c:17]2[cH:18]1
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cnccc23)CC1
c1cc(NC2CCNCC2)c2ccncc2c1
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 32 (327 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cnccc23)CC1>>c1cc(NC2CCNCC2)c2ccncc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-52248c0e52ae41509e95eacfd95e2764
CC(C)(C)OC(=O)N1CCC(CNc2cccc3cnccc23)CC1>>c1cc(NCC2CCNCC2)c2ccncc2c1
C(C)(C)(C)OC(=O)N1CCC(CC1)CNC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NCC1CCNCC1
CC(C)(C)OC(=O)[N:10]1[CH2:9][CH2:8][CH:7]([CH2:6][NH:5][c:4]2[cH:3][cH:2][cH:19][c:18]3[c:13]2[cH:14][cH:15][n:16][cH:17]3)[CH2:12][CH2:11]1>>[cH:2]1[cH:3][c:4]([NH:5][CH2:6][CH:7]2[CH2:8][CH2:9][NH:10][CH2:11][CH2:12]2)[c:13]2[cH:14][cH:15][n:16][cH:17][c:18]2[cH:19]1
CC(C)(C)OC(=O)N1CCC(CNc2cccc3cnccc23)CC1
c1cc(NCC2CCNCC2)c2ccncc2c1
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NCC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 33 (171 mg) and 10% hydrogen chloride/methanol solution (2.5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with m...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(CNc2cccc3cnccc23)CC1>>c1cc(NCC2CCNCC2)c2ccncc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-919d2c5e1db54d07986b3c573f3147b2
CC(C)(C)OC(=O)N1CCCC(CNc2cccc3cnccc23)C1>>c1cc(NCC2CCCNC2)c2ccncc2c1
C(C)(C)(C)OC(=O)N1CC(CCC1)CNC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NCC1CNCCC1
CC(C)(C)OC(=O)[N:11]1[CH2:10][CH2:9][CH2:8][CH:7]([CH2:6][NH:5][c:4]2[cH:3][cH:2][cH:19][c:18]3[c:13]2[cH:14][cH:15][n:16][cH:17]3)[CH2:12]1>>[cH:2]1[cH:3][c:4]([NH:5][CH2:6][CH:7]2[CH2:8][CH2:9][CH2:10][NH:11][CH2:12]2)[c:13]2[cH:14][cH:15][n:16][cH:17][c:18]2[cH:19]1
CC(C)(C)OC(=O)N1CCCC(CNc2cccc3cnccc23)C1
c1cc(NCC2CCCNC2)c2ccncc2c1
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NCC2CCCNC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:5]-[C:4]-[NH;D2;+0:1]-[C:2]-[C:3]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 34 (171 mg) and 10% hydrogen chloride/methanol solution (2.5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with m...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCCC(CNc2cccc3cnccc23)C1>>c1cc(NCC2CCCNC2)c2ccncc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d2ae7ccd3f25492baf70cc5fa51d6131
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](O)CC1.CS(=O)(=O)Cl>>CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](OS(C)(=O)=O)CC1
O.CO.C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)O.CS(=O)(=O)Cl>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OS(=O)(=O)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@H:12]([OH:13])[CH2:18][CH2:19]1.Cl[S:14]([CH3:15])(=[O:16])=[O:17]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@H:12]([O:13][S:14]([CH3:15])(=[O:16])=[O:17])[CH2:18][CH2:19]1
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](O)CC1.CS(=O)(=O)Cl
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](OS(C)(=O)=O)CC1
null
null
N1=CC=CC=C1
Acylation
Formation of Sulfonic Esters
641955d0081c80f158ce2aacd31873a3f3301c87ca0800cf263e288ba8390217
4f9373df8a11470603daf885a5777cebf95940370e32739263d35df0f171a0dd
C1CCCCC1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6](-[OH;D1;+0:7])-[C:8]>>[C:5]-[C:6](-[O;H0;D2;+0:7]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4])-[C:8]
null
[]
null
null
15
MINUTE
A solution of Intermediate 35 (90.3 g) in pyridine (415 ml) was added dropwise with methanesulfonyl chloride (42.4 ml) with stirring and ice cooling over 15 minutes and stirred with ice cooling for 30 minutes and at room temperature for 20 minutes. The reaction mixture was added with methanol (54.2 ml) to terminate the...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Sulfonyl halide
Mesylate
null
null
C1CCCCC1
HCl
N1=CC=CC=C1
null
0.25
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](O)CC1.CS(=O)(=O)Cl>N1=CC=CC=C1>CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](OS(C)(=O)=O)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b811f8e37f91454ca9c82dfe2654d854
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](OS(C)(=O)=O)CC1.C[Si](C)(C)N=[N+]=[N-]>>CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N=[N+]=[N-])CC1
O.C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)OS(=O)(=O)C.C[Si](C)(C)N=[N+]=[N-].[F-].[Cs+]>>C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)N=[N+]=[N-]
CS(=O)(=O)O[C@H:12]1[CH2:11][CH2:10][C@H:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:17][CH2:16]1.C[Si](C)(C)[N:13]=[N+:14]=[N-:15]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@@H:12]([N:13]=[N+:14]=[N-:15])[CH2:16][CH2:17]1
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](OS(C)(=O)=O)CC1.C[Si](C)(C)N=[N+]=[N-]
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N=[N+]=[N-])CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
d3ae5583ed85436d254cdb02077da151826687662d071f700d766a96fefbcdac
07318ec98fcf637ef5b643775774166eb320ca1ca12ae991c23914bca80bab51
C1CCCCC1
C-S(=O)(=O)-O-[C@@H;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5].C-[Si](-C)(-C)-[N;H0;D2;+0:6]=[#7;+:7]=[N;-;D1;H0:8]>>[C:3]-[C:2]-[C@@H;D3;+0:1](-[N;H0;D2;+0:6]=[#7;+:7]=[N;-;D1;H0:8])-[C:4]-[C:5]
null
[]
null
null
null
null
A solution of Intermediate 36 (196 g) and trimethylsilyl azide (283 ml, Tokyo Kasei Kogyo) in dimethylformamide (667 ml) was added with cesium fluoride (305 g, Wako Pure Chemical Industries) with stirring and stirred at 70° C. for 4 days. The reaction mixture was cooled to room temperature and then added twice with wat...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Azide.Silyl protective group
Azide
C1CCCCC1
C1CCCCC1
C1CCCCC1
MsOH.HO-
CN(C=O)C
null
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](OS(C)(=O)=O)CC1.C[Si](C)(C)N=[N+]=[N-]>CN(C=O)C>CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N=[N+]=[N-])CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fea9acd2f75549b088952fd82f2bc28a
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N=[N+]=[N-])CC1>>CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1
C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)N=[N+]=[N-]>>C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)N
[N-]=[N+]=[N:13][C@@H:12]1[CH2:11][CH2:10][C@H:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:15][CH2:14]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@@H:12]([NH2:13])[CH2:14][CH2:15]1
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N=[N+]=[N-])CC1
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1
null
[Pd]
C(C)(=O)OCC
Reduction
Azide to amine reduction (Staudinger)
4c9e4990dae2bb965dec06bd45e318560989ee3681b61e443f7aa363b7cfa222
cd009d687d606bf351eac9390a176d16be38f2c8216a599b398641009c215027
C1CCCCC1
[C:1]-[C:2](-[N;H0;D2;+0:3]=[N+]=[N-])-[C:4]>>[C:1]-[C:2](-[NH2;D1;+0:3])-[C:4]
36.2
[{"value": 36.2, "product": "C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The roughly purified product of Intermediate 37 (142 g) was reduced by hydrogenation at room temperature for 9 hours by using 10% Pd/C (7.1 g) and ethyl acetate solution (1.42 l) under hydrogen atmosphere of 1 atm. The palladium catalyst was removed by filtration, and the solvent was evaporated under reduced pressure. ...
10.6084/m9.figshare.5104873.v1
null
Azide
Primary amine
null
null
C1CCCCC1
Other
[Pd].C(C)(=O)OCC
null
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N=[N+]=[N-])CC1>[Pd].C(C)(=O)OCC>CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-62ca8446a3a044da8763ed93973f3667
Brc1cccc2cnccc12.CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1>>CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
BrC1=C2C=CN=CC2=CC=C1.C(C)(C)(C)P(C1=C(C=CC=C1)C1=CC=CC=C1)C(C)(C)C.C(C)(C)(C)OC(=O)N[C@H]1CC[C@H](CC1)N.CC(C)([O-])C.[Na+]>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)NC1=C2C=CN=CC2=CC=C1
Br[c:14]1[cH:15][cH:16][cH:17][c:18]2[cH:19][n:20][cH:21][cH:22][c:23]12.[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@@H:12]([NH2:13])[CH2:24][CH2:25]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@@H:12]([NH:13][c:14]2[cH:15][cH:16][cH:17][c:18]3[...
Brc1cccc2cnccc12.CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
17c3dbb58f19c559a89452c2c52a32d81319b5dd6d11e225611cc478eba61c1b
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1cc(NC2CCCCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[C:10]-[C:11](-[NH2;D1;+0:12])-[C:13]>>[C:10]-[C:11](-[NH;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1)-[C:13]
77.1
[{"value": 77.1, "product": "C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)NC1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
null
null
Under nitrogen atmosphere, a suspension of 5-bromoisoquinoline (253 mg), tris(dibenzylideneacetone)palladium(0) (58 mg), 2-(di-tert-butylphosphino)biphenyl (74 mg), Intermediate 38 (311 mg) and sodium tert-butoxide (165 mg) in toluene was stirred with heating at 70° C. for 3 hours. The reaction mixture was cooled to ro...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
C1CCCCC1.c1ccc2cnccc2c1
HBr
C1(=CC=CC=C1)C
70
null
Brc1cccc2cnccc12.CC(C)(C)OC(=O)N[C@@H]1CC[C@H](N)CC1>C1(=CC=CC=C1)C>CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8889760d8b024e68bc4a6d002cdc2fe4
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1>>N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@@H](CC1)NC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)N[C@@H]1CC[C@@H](CC1)N
CC(C)(C)OC(=O)[NH:2][C@H:3]1[CH2:4][CH2:5][C@@H:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][cH:16][c:17]23)[CH2:18][CH2:19]1>>[NH2:2][C@H:3]1[CH2:4][CH2:5][C@@H:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][cH:16][c:17]23)[CH2:18][CH2:19]1
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (room temperature, 31 hours) by using Intermediate 39 (214 mg) and 10% hydrogen chloride/methanol solution (5 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (1 ml) and diethyl ether (3 ml). The depo...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1>>N[C@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c614d1288161409291394e06408d3032
Brc1cccc2cnccc12.CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](N)CC1>>CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
BrC1=C2C=CN=CC2=CC=C1.C(C)(C)(C)P(C1=C(C=CC=C1)C1=CC=CC=C1)C(C)(C)C.C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)N.CC(C)([O-])C.[Na+]>>C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)NC1=C2C=CN=CC2=CC=C1
Br[c:14]1[cH:15][cH:16][cH:17][c:18]2[cH:19][n:20][cH:21][cH:22][c:23]12.[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@H:12]([NH2:13])[CH2:24][CH2:25]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@H:9]1[CH2:10][CH2:11][C@H:12]([NH:13][c:14]2[cH:15][cH:16][cH:17][c:18]3[cH...
Brc1cccc2cnccc12.CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](N)CC1
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
17c3dbb58f19c559a89452c2c52a32d81319b5dd6d11e225611cc478eba61c1b
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1cc(NC2CCCCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1.[C:10]-[C:11](-[NH2;D1;+0:12])-[C:13]>>[C:10]-[C:11](-[NH;D2;+0:12]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1)-[C:13]
42
[{"value": 42.0, "product": "C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)NC1=C2C=CN=CC2=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
null
null
Under nitrogen atmosphere, a suspension of 5-bromoisoquinoline (100 mg), tris(dibenzylideneacetone)palladium(0) (23 mg), 2-(di-tert-butylphosphino)biphenyl (29 mg), Intermediate 40 (122 mg) and sodium tert-butoxide (66 mg) in toluene was stirred with heating at 70° C. for 3.5 hours. The reaction mixture was cooled to r...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2cnccc2c1
c1ccc2cnccc2c1
C1CCCCC1.c1ccc2cnccc2c1
HBr
C1(=CC=CC=C1)C
70
null
Brc1cccc2cnccc12.CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](N)CC1>C1(=CC=CC=C1)C>CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b3463dd1e45d4ff9a4d87ab1ddd0da87
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1>>N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
C(C)(C)(C)OC(=O)N[C@@H]1CC[C@H](CC1)NC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)N[C@@H]1CC[C@H](CC1)N
CC(C)(C)OC(=O)[NH:2][C@H:3]1[CH2:4][CH2:5][C@H:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][cH:16][c:17]23)[CH2:18][CH2:19]1>>[NH2:2][C@H:3]1[CH2:4][CH2:5][C@H:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][cH:16][c:17]23)[CH2:18][CH2:19]1
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 1 hour) by using Intermediate 41 (69 mg) and 10% hydrogen chloride/methanol solution (4 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (0.5 ml) and diethyl ether (2 ml). The deposited preci...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1>>N[C@@H]1CC[C@@H](Nc2cccc3cnccc23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4e36bb6d06d14714a6ce9ecc8076eb40
CC(C)(C)OC(=O)NC1CCCC(Nc2cccc3cnccc23)C1>>NC1CCCC(Nc2cccc3cnccc23)C1
C(C)(C)(C)OC(=O)NC1CC(CCC1)NC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NC1CC(CCC1)N
CC(C)(C)OC(=O)[NH:2][CH:3]1[CH2:4][CH2:5][CH2:6][CH:7]([NH:8][c:9]2[cH:10][cH:11][cH:12][c:13]3[cH:14][n:15][cH:16][cH:17][c:18]23)[CH2:19]1>>[NH2:2][CH:3]1[CH2:4][CH2:5][CH2:6][CH:7]([NH:8][c:9]2[cH:10][cH:11][cH:12][c:13]3[cH:14][n:15][cH:16][cH:17][c:18]23)[CH2:19]1
CC(C)(C)OC(=O)NC1CCCC(Nc2cccc3cnccc23)C1
NC1CCCC(Nc2cccc3cnccc23)C1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 43 (171 mg) and 10% hydrogen chloride/methanol solution (2.5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with m...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NC1CCCC(Nc2cccc3cnccc23)C1>>NC1CCCC(Nc2cccc3cnccc23)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c1897e61e42c4a49b6fe74b11d882df6
CC(C)(C)OC(=O)NCc1cccc(CNc2cccc3cnccc23)c1>>NCc1cccc(CNc2cccc3cnccc23)c1
C(C)(C)(C)OC(=O)NCC1=CC(=CC=C1)CNC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)NCC1=CC(=CC=C1)CN
CC(C)(C)OC(=O)[NH:2][CH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]([CH2:9][NH:10][c:11]2[cH:12][cH:13][cH:14][c:15]3[cH:16][n:17][cH:18][cH:19][c:20]23)[cH:21]1>>[NH2:2][CH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]([CH2:9][NH:10][c:11]2[cH:12][cH:13][cH:14][c:15]3[cH:16][n:17][cH:18][cH:19][c:20]23)[cH:21]1
CC(C)(C)OC(=O)NCc1cccc(CNc2cccc3cnccc23)c1
NCc1cccc(CNc2cccc3cnccc23)c1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccc(CNc2cccc3cnccc23)cc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[c:3]>>[NH2;D1;+0:1]-[C:2]-[c:3]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 44 (364 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NCc1cccc(CNc2cccc3cnccc23)c1>>NCc1cccc(CNc2cccc3cnccc23)c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-165bb2fd30774dcab9791f3bb61ece03
CC(C)(C)OC(=O)N1CCC(Oc2cccc3cnccc23)CC1>>c1cc(OC2CCNCC2)c2ccncc2c1
C(C)(C)(C)OC(=O)N1CCC(CC1)OC1=C2C=CN=CC2=CC=C1.Cl.CO>>Cl.C1=NC=CC2=C(C=CC=C12)OC1CCNCC1
CC(C)(C)OC(=O)[N:9]1[CH2:8][CH2:7][CH:6]([O:5][c:4]2[cH:3][cH:2][cH:18][c:17]3[c:12]2[cH:13][cH:14][n:15][cH:16]3)[CH2:11][CH2:10]1>>[cH:2]1[cH:3][c:4]([O:5][CH:6]2[CH2:7][CH2:8][NH:9][CH2:10][CH2:11]2)[c:12]2[cH:13][cH:14][n:15][cH:16][c:17]2[cH:18]1
CC(C)(C)OC(=O)N1CCC(Oc2cccc3cnccc23)CC1
c1cc(OC2CCNCC2)c2ccncc2c1
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(OC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 45 (164 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(Oc2cccc3cnccc23)CC1>>c1cc(OC2CCNCC2)c2ccncc2c1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d468fd2f35634bbfb59c0f3c2c17ef5c
CC(C)(C)OC(=O)N1CCC(=O)CC1.CN>>CC(C)(C)OC(=O)N1CCC(CN)CC1
Cl.CN.C(C)(C)(C)OC(=O)N1CCC(CC1)=O>>NCC1CCN(CC1)C(=O)OC(C)(C)C
O=[C:11]1[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:15][CH2:14]1.[CH3:12][NH2:13]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][NH2:13])[CH2:14][CH2:15]1
CC(C)(C)OC(=O)N1CCC(=O)CC1.CN
CC(C)(C)OC(=O)N1CCC(CN)CC1
null
[Pt]=O
CO
C-C Coupling
OtherReaction
14bcc3d5cb0dcac5a2469be26468af2477782b3701e5498fcf8d7c85badaa1c1
06a42e352cf517302d592bf38a2fd11b220014e39071074dc7becb6ee0bee4b2
C1CCNCC1
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1.[CH3;D1;+0:7]-[N;D1;H2:8]>>[N;D1;H2:8]-[CH2;D2;+0:7]-[CH;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1
93.9
[{"value": 93.9, "product": "NCC1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of methylamine hydrochloride (1.01 g, Wako Pure Chemical Industries) and 1-(tert-butoxycarbonyl)-4-oxopiperidine (1.99 g, Aldrich) in methanol (13 ml) was stirred in the presence of platinum oxide (69 mg, Wako Pure Chemical Industries) at room temperature for 3 hours under hydrogen atmosphere of ordinary pre...
10.6084/m9.figshare.5104873.v1
null
Ketone
null
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1
Other
[Pt]=O.CO
null
null
CC(C)(C)OC(=O)N1CCC(=O)CC1.CN>[Pt]=O.CO>CC(C)(C)OC(=O)N1CCC(CN)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c2cdce0bfcd242c092bbc9b6cdab22de
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1>>Brc1cncc2cccc(NC3CCNCC3)c12
BrC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.BrC1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:15]1[CH2:14][CH2:13][CH:12]([NH:11][c:10]2[cH:9][cH:8][cH:7][c:6]3[cH:5][n:4][cH:3][c:2]([Br:1])[c:18]32)[CH2:17][CH2:16]1>>[Br:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][CH:12]3[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]3)[c:18]12
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1
Brc1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 71 (123 mg) and 10% hydrogen chloride/methanol solution (6 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1>>Brc1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-da4afad36c4f493fbe7676c2dafd28c1
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.[F-]>>CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(F)c23)CC1
BrC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.[F-].[Cs+]>>FC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C
Br[c:21]1[cH:20][n:19][cH:18][c:17]2[cH:16][cH:15][cH:14][c:13]([NH:12][CH:11]3[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:25][CH2:24]3)[c:23]21.[F-:22]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([NH:12][c:13]2[cH:14][cH:15][cH:16][c:17]3[cH:18][n:19][cH...
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.[F-]
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(F)c23)CC1
null
null
CS(=O)C
Functional Group Interconversion
OtherReaction
aa78c0e2316a6dfe08001566d0f24f6ef11c0313c23f6e9a699dc1e464209d61
4131cd1655d0ec8ecf7e181a36ab37eb3293d734e38ece0acf0e59405d170401
c1cc(NC2CCNCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7].[F-;H0;D0:8]>>[F;H0;D1;+0:8]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
23.9
[{"value": 23.9, "product": "FC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
150
CELSIUS
8
HOUR
A solution of Intermediate 71 (104 mg) in dimethyl sulfoxide (2 ml) was added with cesium fluoride (284 mg, Wako Pure Chemical Industries) and stirred at 150° C. for 8 hours. The reaction mixture was cooled to room temperature and then filtered through Celite. The residue was added with water (20 ml), extracted with et...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Aromatic halide
c1ccc2cnccc2c1
c1ccc2cnccc2c1
C1CC[NH]CC1.c1ccc2cnccc2c1
Br-
CS(=O)C
150
8
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.[F-]>CS(=O)C>CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(F)c23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c17282f2eff94c059e2a09b237b7e77a
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(F)c23)CC1>>Fc1cncc2cccc(NC3CCNCC3)c12
FC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.FC1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([F:2])[c:19]32)[CH2:18][CH2:17]1>>[F:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)[c:19]12
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(F)c23)CC1
Fc1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 72 (30.2 mg) and 10% hydrogen chloride/methanol solution (3 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(F)c23)CC1>>Fc1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-daedd6bee30f484fb7b742c746a69337
CSc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>CSc1cncc2cccc(NC3CCNCC3)c12
CSC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.CSC1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([S:2][CH3:1])[c:19]32)[CH2:18][CH2:17]1>>[CH3:1][S:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)[c:19]12
CSc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
CSc1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 74 (214 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
CSc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>CSc1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2e9115487cd940a38efae8fd5e24df8a
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.Cc1cc(C(C)(C)C)c(O)c(C(C)(C)C)c1>>Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
BrC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.C[Sn](C)(C)C.C(C)(C)(C)C1=C(C(=CC(=C1)C)C(C)(C)C)O>>CC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C
Br[c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][CH:12]3[CH2:13][CH2:14][N:15]([C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])[CH2:23][CH2:24]3)[c:25]12.CC(C)(C)c1cc([CH3:1])cc(C(C)(C)C)c1O>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][CH:12]3[CH2:13][CH2:14][N:15]([C:16]...
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.Cc1cc(C(C)(C)C)c(O)c(C(C)(C)C)c1
Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
null
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1
C1(=CC=CC=C1)C
C-C Coupling
OtherReaction
97910f5eb556ac900e7b376fa52c06a18456b9862405e525f85d744e9ca92a9d
65063d04424efe73d77012373052a6459d6dbe14093a552d44836b582c9a5c53
c1cc(NC2CCNCC2)c2ccncc2c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7].C-C(-C)(-C)-c1:c:c(-[CH3;D1;+0:8]):c:c(-C(-C)(-C)-C):c:1-O>>[CH3;D1;+0:8]-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1:[c:7]
null
[]
150
CELSIUS
48
HOUR
A solution of Intermediate 71 (313 mg) in toluene (6 ml) was added with tetrakis(triphenylphosphine)palladium(0) (17.9 mg, Aldrich), tetramethyltin (165 μl, Kanto Chemicals) and 2,6-di-tert-butyl-4-methylphenol (several pellets, Tokyo Kasei Kogyo) and stirred in a sealed tube at 150° C. for 48 hours. The reaction mixtu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic alcohol
null
c1ccc2cnccc2c1.c1ccccc1
c1ccc2cnccc2c1
c1ccc2cnccc2c1.C1CC[NH]CC1
HBr
C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.C1(=CC=CC=C1)C
150
48
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(Br)c23)CC1.Cc1cc(C(C)(C)C)c(O)c(C(C)(C)C)c1>C=1C=CC(=CC1)[P](C=2C=CC=CC2)(C=3C=CC=CC3)[Pd]([P](C=4C=CC=CC4)(C=5C=CC=CC5)C=6C=CC=CC6)([P](C=7C=CC=CC7)(C=8C=CC=CC8)C=9C=CC=CC9)[P](C=1C=CC=CC1)(C=1C=CC=CC1)C=1C=CC=CC1.C1(=CC=CC=C1)C>Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b671ee9a0ae746f496e932de4e8b9c07
Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(NC3CCNCC3)c12
CC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.CC1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:15]1[CH2:14][CH2:13][CH:12]([NH:11][c:10]2[cH:9][cH:8][cH:7][c:6]3[cH:5][n:4][cH:3][c:2]([CH3:1])[c:18]32)[CH2:17][CH2:16]1>>[CH3:1][c:2]1[cH:3][n:4][cH:5][c:6]2[cH:7][cH:8][cH:9][c:10]([NH:11][CH:12]3[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]3)[c:18]12
Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
Cc1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 75 (90.7 mg) and 10% hydrogen chloride/methanol solution (2 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>Cc1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-50d3985a248b4699b78cd3135ee56178
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Br)c23)CC1>>NC1CCC(Nc2cccc3cncc(Br)c23)CC1
C(C)(C)(C)OC(=O)NC1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)Br.Cl.CO>>Cl.BrC1=CN=CC2=CC=CC(=C12)NC1CCC(CC1)N
CC(C)(C)OC(=O)[NH:2][CH:3]1[CH2:4][CH2:5][CH:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][c:16]([Br:17])[c:18]23)[CH2:19][CH2:20]1>>[NH2:2][CH:3]1[CH2:4][CH2:5][CH:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][c:16]([Br:17])[c:18]23)[CH2:19][CH2:20]1
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Br)c23)CC1
NC1CCC(Nc2cccc3cncc(Br)c23)CC1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 76 (124 mg) and 10% hydrogen chloride/methanol solution (3 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(Br)c23)CC1>>NC1CCC(Nc2cccc3cncc(Br)c23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-111ff57987e04934a9f32b32aff15edd
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(F)c23)CC1>>NC1CCC(Nc2cccc3cncc(F)c23)CC1
C(C)(C)(C)OC(=O)NC1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)F.Cl.CO>>Cl.FC1=CN=CC2=CC=CC(=C12)NC1CCC(CC1)N
CC(C)(C)OC(=O)[NH:2][CH:3]1[CH2:4][CH2:5][CH:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][c:16]([F:17])[c:18]23)[CH2:19][CH2:20]1>>[NH2:2][CH:3]1[CH2:4][CH2:5][CH:6]([NH:7][c:8]2[cH:9][cH:10][cH:11][c:12]3[cH:13][n:14][cH:15][c:16]([F:17])[c:18]23)[CH2:19][CH2:20]1
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(F)c23)CC1
NC1CCC(Nc2cccc3cncc(F)c23)CC1
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 77 (90.8 mg) and 10% hydrogen chloride/methanol solution (2 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CCCCC1.c1ccc2cnccc2c1
HO-
null
null
null
CC(C)(C)OC(=O)NC1CCC(Nc2cccc3cncc(F)c23)CC1>>NC1CCC(Nc2cccc3cncc(F)c23)CC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b59867340aaa44959c4661c4e65259c3
CSc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12>>CSc1cncc2cccc(NC3CCC(N)CC3)c12
C(C)(C)(C)OC(=O)NC1CCC(CC1)NC1=C2C(=CN=CC2=CC=C1)SC.Cl.CO>>Cl.CSC1=CN=CC2=CC=CC(=C12)NC1CCC(CC1)N
CC(C)(C)OC(=O)[NH:17][CH:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([S:2][CH3:1])[c:20]32)[CH2:19][CH2:18]1>>[CH3:1][S:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][CH:16]([NH2:17])[CH2:18][CH2:19]3)[c:20]12
CSc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12
CSc1cncc2cccc(NC3CCC(N)CC3)c12
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1cc(NC2CCCCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 78 (341 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccc2cnccc2c1.C1CCCCC1
HO-
null
null
null
CSc1cncc2cccc(NC3CCC(NC(=O)OC(C)(C)C)CC3)c12>>CSc1cncc2cccc(NC3CCC(N)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-43fad62811f54559b279903164b86c04
CSc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12.OO>>CS(=O)c1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
CSC1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.C(C)(=O)O.OO>>CS(=O)C1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C
[CH3:1][S:2][c:4]1[cH:5][n:6][cH:7][c:8]2[cH:9][cH:10][cH:11][c:12]([NH:13][CH:14]3[CH2:15][CH2:16][N:17]([C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[CH2:25][CH2:26]3)[c:27]12.O[OH:3]>>[CH3:1][S:2](=[O:3])[c:4]1[cH:5][n:6][cH:7][c:8]2[cH:9][cH:10][cH:11][c:12]([NH:13][CH:14]3[CH2:15][CH2:16][N:17]([C:18](=...
CSc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12.OO
CS(=O)c1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
null
null
C(C)(=O)OCC
Oxidation
Sulfanyl to sulfinyl_H2O2
3f94fa67dce0f9d1622f25c2f6b679e0a2528e6d5c5559b15aed37456745a4b5
099322fb111e24ec324e6fad75d493a762ca0cd5af0df8c6f3bfd25c910b45a8
c1cc(NC2CCNCC2)c2ccncc2c1
O-[OH;D1;+0:1].[C;D1;H3:2]-[S;H0;D2;+0:3]-[c:4](:[c:5]):[c:6]:[#7;a:7]:[c:8]>>[C;D1;H3:2]-[S;H0;D3;+0:3](=[O;H0;D1;+0:1])-[c:4](:[c:5]):[c:6]:[#7;a:7]:[c:8]
null
[]
null
null
17
HOUR
Intermediate 74 (746 mg) obtained in Example 105, Step B was added with acetic acid (1.5 ml) and 30% aqueous hydrogen peroxide (2 ml) and stirred at room temperature for 17 hours. The reaction mixture was added with ethyl acetate (50 ml) and washed three times with saturated aqueous sodium hydrogencarbonate (25 ml for ...
10.6084/m9.figshare.5104873.v1
null
Peroxide.Monosulfide
Sulfoxide
null
null
c1ccc2cnccc2c1.C1CC[NH]CC1
HO-
C(C)(=O)OCC
null
17
CSc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12.OO>C(C)(=O)OCC>CS(=O)c1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6fb0dd10e1f9415d9ffb3aac8812cd63
CS(=O)c1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>CS(=O)c1cncc2cccc(NC3CCNCC3)c12
CS(=O)C1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.CS(=O)C1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:17]1[CH2:16][CH2:15][CH:14]([NH:13][c:12]2[cH:11][cH:10][cH:9][c:8]3[cH:7][n:6][cH:5][c:4]([S:2]([CH3:1])=[O:3])[c:20]32)[CH2:19][CH2:18]1>>[CH3:1][S:2](=[O:3])[c:4]1[cH:5][n:6][cH:7][c:8]2[cH:9][cH:10][cH:11][c:12]([NH:13][CH:14]3[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]3)[c:20]12
CS(=O)c1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
CS(=O)c1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 79 (138 mg) and 10% hydrogen chloride/methanol solution (3 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with met...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
CS(=O)c1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>CS(=O)c1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5f8fc3e5b08c415e8eb79577e5b04040
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(S(C)(=O)=O)c23)CC1>>CS(=O)(=O)c1cncc2cccc(NC3CCNCC3)c12
CS(=O)(=O)C1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.CS(=O)(=O)C1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:18]1[CH2:17][CH2:16][CH:15]([NH:14][c:13]2[cH:12][cH:11][cH:10][c:9]3[cH:8][n:7][cH:6][c:5]([S:2]([CH3:1])(=[O:3])=[O:4])[c:21]32)[CH2:20][CH2:19]1>>[CH3:1][S:2](=[O:3])(=[O:4])[c:5]1[cH:6][n:7][cH:8][c:9]2[cH:10][cH:11][cH:12][c:13]([NH:14][CH:15]3[CH2:16][CH2:17][NH:18][CH2:19][CH2:20]3)[c:21]12
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(S(C)(=O)=O)c23)CC1
CS(=O)(=O)c1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 80 (40.9 mg) and 10% hydrogen chloride/methanol solution (1 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3cncc(S(C)(=O)=O)c23)CC1>>CS(=O)(=O)c1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dd7fd85d74ac4d629c9b080664ed5570
C=Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>C=Cc1cncc2cccc(NC3CCNCC3)c12
C(=C)C1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.C(=C)C1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([CH:2]=[CH2:1])[c:19]32)[CH2:18][CH2:17]1>>[CH2:1]=[CH:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)[c:19]12
C=Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
C=Cc1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 81 (46.6 mg) and 10% hydrogen chloride/methanol solution (2 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
C=Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>C=Cc1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-33f191967e254d3f863ca6e7e74696a6
C=Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>CCc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
C(=C)C1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C>>C(C)C1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C
[CH2:1]=[CH:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][N:16]([C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[CH2:24][CH2:25]3)[c:26]12>>[CH3:1][CH2:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][N:16]([C:17](=[O:18])[O:19][...
C=Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
CCc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
null
[C].[Pd]
CO
Reduction
Hydrogenation (double to single)
8276b4fb5ddc7d15dec6d92474e91e2dbb2fb8b81e5b5720762e5d89cb27aa69
1ccae9f2e86499601fc3421041ff4588c8e6fd53048e86c3b6ed12ae873609c0
c1cc(NC2CCNCC2)c2ccncc2c1
[CH2;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[CH3;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
90.5
[{"value": 90.5, "product": "C(C)C1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution (2 ml) of Intermediate 81 (103 mg) in methanol was vigorously stirred in the presence of 10% palladium carbon catalyst (16.5 mg) at room temperature under hydrogen atmosphere of ordinary pressure. The reaction mixture was filtered through Celite, and the solvent was evaporated under reduced pressure. The res...
10.6084/m9.figshare.5104873.v1
null
Vinyl
null
null
null
c1ccc2cnccc2c1.C1CC[NH]CC1
null
[C].[Pd].CO
null
null
C=Cc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>[C].[Pd].CO>CCc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-749ac926d34d4575ae04f26fcd6095f9
CCc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>CCc1cncc2cccc(NC3CCNCC3)c12
C(C)C1=CN=CC2=CC=CC(=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.Cl.CO>>Cl.C(C)C1=CN=CC2=CC=CC(=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:16]1[CH2:15][CH2:14][CH:13]([NH:12][c:11]2[cH:10][cH:9][cH:8][c:7]3[cH:6][n:5][cH:4][c:3]([CH2:2][CH3:1])[c:19]32)[CH2:18][CH2:17]1>>[CH3:1][CH2:2][c:3]1[cH:4][n:5][cH:6][c:7]2[cH:8][cH:9][cH:10][c:11]([NH:12][CH:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)[c:19]12
CCc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12
CCc1cncc2cccc(NC3CCNCC3)c12
null
null
null
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 82 (93.7 mg) and 10% hydrogen chloride/methanol solution (2 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with me...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccc2cnccc2c1.C1CCNCC1
HO-
null
null
null
CCc1cncc2cccc(NC3CCN(C(=O)OC(C)(C)C)CC3)c12>>CCc1cncc2cccc(NC3CCNCC3)c12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c2c568e79a76424c86ebc38f97226234
O=[N+]([O-])c1cccc2c(Cl)nccc12>>Nc1cccc2c(Cl)nccc12
O.O.[Sn](Cl)Cl.ClC1=NC=CC2=C(C=CC=C12)[N+](=O)[O-]>>ClC1=NC=CC2=C(C=CC=C12)N
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][cH:5][c:6]2[c:7]([Cl:8])[n:9][cH:10][cH:11][c:12]12>>[NH2:1][c:2]1[cH:3][cH:4][cH:5][c:6]2[c:7]([Cl:8])[n:9][cH:10][cH:11][c:12]12
O=[N+]([O-])c1cccc2c(Cl)nccc12
Nc1cccc2c(Cl)nccc12
null
null
C(C)(=O)OCC
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc2cnccc2c1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
70
CELSIUS
null
null
A solution (40 ml) of 1-chloro-5-nitroisoquinoline (2.23 g, synthesized according to the method described in J. Med. Chem. 45, 3, 740 (2002)) in ethyl acetate was added with tin(II) chloride dihydrate (12.39 g, Wako Pure Chemical Industries) at room temperature and stirred with heating at 70° C. for 1 hour. The reactio...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2cnccc2c1
Other
C(C)(=O)OCC
70
null
O=[N+]([O-])c1cccc2c(Cl)nccc12>C(C)(=O)OCC>Nc1cccc2c(Cl)nccc12
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c7ab94fd6f5a4dc4b97d834fc0e5f2b3
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1>>Clc1nccc2c(NC3CCNCC3)cccc12
ClC1=NC=CC2=C(C=CC=C12)NC1CCN(CC1)C(=O)OC(C)(C)C.FC(C(=O)O)(F)F>>FC(C(=O)O)(F)F.ClC1=NC=CC2=C(C=CC=C12)NC1CCNCC1
CC(C)(C)OC(=O)[N:12]1[CH2:11][CH2:10][CH:9]([NH:8][c:7]2[c:6]3[cH:5][cH:4][n:3][c:2]([Cl:1])[c:18]3[cH:17][cH:16][cH:15]2)[CH2:14][CH2:13]1>>[Cl:1][c:2]1[n:3][cH:4][cH:5][c:6]2[c:7]([NH:8][CH:9]3[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]3)[cH:15][cH:16][cH:17][c:18]12
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1
Clc1nccc2c(NC3CCNCC3)cccc12
null
null
C(Cl)Cl
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1cc(NC2CCNCC2)c2ccncc2c1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
null
[]
null
null
null
null
Deprotection was performed (room temperature, 2 hours) by using Intermediate 84 (81.9 mg) and a mixed solution of trifluoroacetic acid and methylene chloride (1:1, 2 ml). The solvent was evaporated under reduced pressure, and the residue was added with methanol (2 ml) and diethyl ether (6 ml). The deposited precipitate...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1.c1ccc2cnccc2c1
HO-
C(Cl)Cl
null
null
CC(C)(C)OC(=O)N1CCC(Nc2cccc3c(Cl)nccc23)CC1>C(Cl)Cl>Clc1nccc2c(NC3CCNCC3)cccc12