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-a33f3b286a854755b162b6197f8b9f3f
CC(C)(C)OC(=O)Nn1c(=O)c2cc(F)c(F)c(Cl)c2n(C2CC2)c1=O.CNC1CCNC1.CS(=O)(=O)Cl>>CC(C)(C)OC(=O)Nn1c(=O)c2cc(F)c(N3CCC(CNS(C)(=O)=O)C3)c(Cl)c2n(C2CC2)c1=O
C(C)(C)(C)OC(NN1C(N(C2=C(C(=C(C=C2C1=O)F)F)Cl)C1CC1)=O)=O.N1CC(CC1)NC.C(C)N(CC)CC.C(C)N(CC)CC.CS(=O)(=O)Cl>>C(C)(C)(C)OC(NN1C(N(C2=C(C(=C(C=C2C1=O)F)N1CC(CC1)CNS(=O)(=O)C)Cl)C1CC1)=O)=O
F[c:16]1[c:14]([F:15])[cH:13][c:12]2[c:10](=[O:11])[n:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[c:35](=[O:36])[n:31]([CH:32]3[CH2:33][CH2:34]3)[c:30]2[c:28]1[Cl:29].[NH:17]1[CH2:18][CH2:19][CH:20]([NH:22][CH3:21])[CH2:27]1.Cl[S:23]([CH3:24])(=[O:25])=[O:26]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O...
CC(C)(C)OC(=O)Nn1c(=O)c2cc(F)c(F)c(Cl)c2n(C2CC2)c1=O.CNC1CCNC1.CS(=O)(=O)Cl
CC(C)(C)OC(=O)Nn1c(=O)c2cc(F)c(N3CCC(CNS(C)(=O)=O)C3)c(Cl)c2n(C2CC2)c1=O
null
null
C(C)(=O)OCC.C(C)#N
Acylation
OtherReaction
e8dcfd63826a349914b82e06ab88b34ebbfb0ac921b034f582f6984393e34140
619e998b2d3a1fadc60f9908b52a775399d64f49a596f029e05a5589de6f1026
O=c1[nH]c(=O)n(C2CC2)c2cc(N3CCCC3)ccc12
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].F-[c;H0;D3;+0:5]1:[c:6](-[F;D1;H0:7]):[c:8]:[c:9]2:[c:10]:[#7;a:11]:[c:12]:[#7;a:13](-[C:14]):[c:15]:2:[c:16]:1-[Cl;D1;H0:17].[CH3;D1;+0:18]-[NH;D2;+0:19]-[CH;D3;+0:20]1-[C:21]-[C:22]-[NH;D2;+0:23]-[C:24]-1>>[C:14]-[#7;a:13]1:[c:12]:[#7;a:11]:[c:10]:[c:9]2:[c:8]...
8.4
[{"value": 8.4, "product": "C(C)(C)(C)OC(NN1C(N(C2=C(C(=C(C=C2C1=O)F)N1CC(CC1)CNS(=O)(=O)C)Cl)C1CC1)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A solution of (8-chloro-1-cyclopropyl-6,7-difluoro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)carbamic acid tert-butyl ester (Example 14, 0.37 g, 0.97 mmol) in acetonitrile (20 mL) is added pyrrolidin-3-yl-methylamine (0.115 g, 1.16 mmol) and triethylamine (2.7 mL, 19.3 mmol). After refluxing for 20 hours, the reaction m...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine.Secondary amine.Sulfonyl halide
Sulfonamide.Tertiary amine
c1ccc2ncncc2c1.C1CCNC1
c1ccc2ncncc2c1.C1CC[NH]C1
c1ccc2ncncc2c1.C1CC[NH]C1.C1CC1
HF
C(C)(=O)OCC.C(C)#N
null
2
CC(C)(C)OC(=O)Nn1c(=O)c2cc(F)c(F)c(Cl)c2n(C2CC2)c1=O.CNC1CCNC1.CS(=O)(=O)Cl>C(C)(=O)OCC.C(C)#N>CC(C)(C)OC(=O)Nn1c(=O)c2cc(F)c(N3CCC(CNS(C)(=O)=O)C3)c(Cl)c2n(C2CC2)c1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1a920b8fb152448dab5ca2e70769c5b9
CCOC(=O)C1CN(Cc2ccccc2)CC12CC2>>CC(=O)C1CN(Cc2ccccc2)CC12CC2
C(C)OC(=O)C1CN(CC12CC2)CC2=CC=CC=C2.C[Li]>>C(C1=CC=CC=C1)N1CC2(CC2)C(C1)C(C)=O
CCO[C:2](=[O:3])[CH:4]1[CH2:5][N:6]([CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[CH2:14][C:15]12[CH2:16][CH2:17]2>>[CH3:1][C:2](=[O:3])[CH:4]1[CH2:5][N:6]([CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[CH2:14][C:15]12[CH2:16][CH2:17]2
CCOC(=O)C1CN(Cc2ccccc2)CC12CC2
CC(=O)C1CN(Cc2ccccc2)CC12CC2
null
null
C(C)OCC
Functional Group Interconversion
OtherReaction
600d91131af1bb1ee8c20c567e56234839eb0602aa06d3adc0666216769f9a6a
ebe855e3c62a5d82c9c1d005e3b3e8a9e3b63aca37bc8a601a136cf86007489d
c1ccc(CN2CCC3(CC3)C2)cc1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])-[C:5]-[#7:6]>>[#7:6]-[C:5]-[C:3](-[C;H0;D3;+0:1](-[C;D1;H3:7])=[O;D1;H0:2])-[C:4]
54.6
[{"value": 54.6, "product": "C(C1=CC=CC=C1)N1CC2(CC2)C(C1)C(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-10
CELSIUS
1
HOUR
A solution (−78° C.) of 5-benzyl-5-azaspiro[2.4]heptane-7-carboxylic acid ethyl ester (Example A1a, 8.15 g, 31.4 mmol) in diethyl ether (200 mL) under a nitrogen atmosphere is treated with methyllithium (1.4 M in diethyl ether, 22.4 mL, 31.4 mmol) over a period of 10 minutes. After 1 hour, reaction mixture is warmed to...
10.6084/m9.figshare.5104873.v1
null
Ester
Ketone
null
null
c1ccccc1.C1CC2(CC2)C[NH]1
HO-
C(C)OCC
-10
1
CCOC(=O)C1CN(Cc2ccccc2)CC12CC2>C(C)OCC>CC(=O)C1CN(Cc2ccccc2)CC12CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-eebca15bfe1a40339125a48548988faa
CC(=O)C1CN(Cc2ccccc2)CC12CC2.NO>>CC(=NO)C1CN(Cc2ccccc2)CC12CC2
C(C1=CC=CC=C1)N1CC2(CC2)C(C1)C(C)=O.Cl.NO>>C(C1=CC=CC=C1)N1CC2(CC2)C(C1)C(C)=NO
O=[C:2]([CH3:1])[CH:5]1[CH2:6][N:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15][C:16]12[CH2:17][CH2:18]2.[NH2:3][OH:4]>>[CH3:1][C:2](=[N:3][OH:4])[CH:5]1[CH2:6][N:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15][C:16]12[CH2:17][CH2:18]2
CC(=O)C1CN(Cc2ccccc2)CC12CC2.NO
CC(=NO)C1CN(Cc2ccccc2)CC12CC2
null
null
C(C)(=O)OCC.N1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
b5fd91d879f097d0ef2e8e2d3ef7d2ef0195968870a9602a47b8324c601790b9
1a0ef15294bdb221fb8888b5d4c7fcf00473b11e53da288791d32747daa48d23
c1ccc(CN2CCC3(CC3)C2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[C:3](-[C:4])-[C:5]-[#7:6].[NH2;D1;+0:7]-[O;D1;H1:8]>>[#7:6]-[C:5]-[C:3](-[C;H0;D3;+0:1](-[C;D1;H3:2])=[N;H0;D2;+0:7]-[O;D1;H1:8])-[C:4]
73.5
[{"value": 73.5, "product": "C(C1=CC=CC=C1)N1CC2(CC2)C(C1)C(C)=NO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
1-(5-benzyl-5-azaspiro[2.4]hept-7-yl)ethanone (Example A2a, 3.93 g, 17.1 mmol) and hydroxylamine hydrochloride (1.78 g, 25.7 mmol) are stirred in pyridine (10 mL) at 90° C. After 20 hours, the reaction mixture is diluted with ethyl acetate and the organic layer is washed with saturated NaHCO3, water, and brine. The org...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
Oxime
null
null
c1ccccc1.C1CC2(CC2)C[NH]1
HO-
C(C)(=O)OCC.N1=CC=CC=C1
null
20
CC(=O)C1CN(Cc2ccccc2)CC12CC2.NO>C(C)(=O)OCC.N1=CC=CC=C1>CC(=NO)C1CN(Cc2ccccc2)CC12CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c97a1145efa84e81865b68656041089c
CC(NC(=O)OC(C)(C)C)C1CN(Cc2ccccc2)CC12CC2>>CC(NC(=O)OC(C)(C)C)C1CNCC12CC2
C(C)(C)(C)OC(NC(C)C1CN(CC12CC2)CC2=CC=CC=C2)=O.[H][H]>>C(C)(C)(C)OC(NC(C)C1CNCC12CC2)=O
c1ccc(C[N:13]2[CH2:12][CH:11]([CH:2]([CH3:1])[NH:3][C:4](=[O:5])[O:6][C:7]([CH3:8])([CH3:9])[CH3:10])[C:15]3([CH2:14]2)[CH2:16][CH2:17]3)cc1>>[CH3:1][CH:2]([NH:3][C:4](=[O:5])[O:6][C:7]([CH3:8])([CH3:9])[CH3:10])[CH:11]1[CH2:12][NH:13][CH2:14][C:15]12[CH2:16][CH2:17]2
CC(NC(=O)OC(C)(C)C)C1CN(Cc2ccccc2)CC12CC2
CC(NC(=O)OC(C)(C)C)C1CNCC12CC2
null
[Pd]
CO
Deprotection
Hydrogenolysis of tertiary amines
9cf6addfef11f51b635125d0004c52838eb3e9b3bdcfd23e0798327b9efabf21
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
C1CC2(CC2)CN1
C(-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1)-c1:c:c:c:c:c:1>>[C:3]1-[C:2]-[NH;D2;+0:1]-[C:5]-[C:4]-1
null
[]
null
null
null
null
A solution of [1-(5-benzyl-5-azaspiro[2.4]hept-7-yl)ethyl]carbamic acid tert-butyl ester (Example A4a, 1.47 g) in methanol (30 mL) in a Parr shaker is treated with 10% palladium on carbon (0.5 g) and hydrogen introduced (50 psi) for 24 hours. The reaction mixture is filtered through celite, washed with methanol, and th...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.C1CC2(CC2)C[NH]1
C1CC2(CC2)CN1
C1CC2(CC2)CN1
Other
[Pd].CO
null
null
CC(NC(=O)OC(C)(C)C)C1CN(Cc2ccccc2)CC12CC2>[Pd].CO>CC(NC(=O)OC(C)(C)C)C1CNCC12CC2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-03179abb6e0a461e9c57bc862974a3e0
NO.O=C1CCN(Cc2ccccc2)C1>>ON=C1CCN(Cc2ccccc2)C1
C(C1=CC=CC=C1)N1CC(CC1)=O.Cl.NO>>C(C1=CC=CC=C1)N1CC(CC1)=NO
[OH:1][NH2:2].O=[C:3]1[CH2:4][CH2:5][N:6]([CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[CH2:14]1>>[OH:1][N:2]=[C:3]1[CH2:4][CH2:5][N:6]([CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[CH2:14]1
NO.O=C1CCN(Cc2ccccc2)C1
ON=C1CCN(Cc2ccccc2)C1
null
null
C(C)(=O)OCC.N1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
916d29c6e2842769ff58df57caef65bf8c6f49de29ec4bf15f1f69069996ca57
1a0ef15294bdb221fb8888b5d4c7fcf00473b11e53da288791d32747daa48d23
N=C1CCN(Cc2ccccc2)C1
O=[C;H0;D3;+0:1]1-[C:2]-[#7:3](-[C:4])-[C:5]-[C:6]-1.[NH2;D1;+0:7]-[O;D1;H1:8]>>[C:4]-[#7:3]1-[C:2]-[C;H0;D3;+0:1](=[N;H0;D2;+0:7]-[O;D1;H1:8])-[C:6]-[C:5]-1
102.2
[{"value": 102.2, "product": "C(C1=CC=CC=C1)N1CC(CC1)=NO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
90
CELSIUS
5
HOUR
To a solution of 1-benzylpyrrolidin-3-one (1.0 g, 5.71 mmol) in pyridine (5 mL) is added hydroxylamine hydrochloride (0.59 g, 8.57 mmol). After stirring at 90° C. for 5 hours, the reaction mixture is diluted with ethyl acetate and washed with saturated sodium bicarbonate, water, and brine. The organic layer is dried ov...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
Oxime
C1CC[NH]C1
C1CC[NH]C1
C1CC[NH]C1.c1ccccc1
HO-
C(C)(=O)OCC.N1=CC=CC=C1
90
5
NO.O=C1CCN(Cc2ccccc2)C1>C(C)(=O)OCC.N1=CC=CC=C1>ON=C1CCN(Cc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2c40f5f2214f4dffa7218b5f4c2a3986
CC=C1CCN(C(=O)OCc2ccccc2)C1>>CC1OC12CCN(C(=O)OCc1ccccc1)C2
C(C1=CC=CC=C1)OC(=O)N1CC(CC1)=CC.ClC=1C=C(C(=O)OO)C=CC1.S(=O)([O-])[O-].[Na+].[Na+]>>C(C1=CC=CC=C1)OC(=O)N1CC2(C(O2)C)CC1
[CH3:1][CH:2]=[C:4]1[CH2:5][CH2:6][N:7]([C:8](=[O:9])[O:10][CH2:11][c:12]2[cH:13][cH:14][cH:15][cH:16][cH:17]2)[CH2:18]1>>[CH3:1][CH:2]1[O:3][C:4]12[CH2:5][CH2:6][N:7]([C:8](=[O:9])[O:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1)[CH2:18]2
CC=C1CCN(C(=O)OCc2ccccc2)C1
CC1OC12CCN(C(=O)OCc1ccccc1)C2
null
null
ClCCl
Oxidation
OtherReaction
9e5cb6df82d89bae604c84d21c7e428abe38ca213049c31d702e54f4902a8523
064ea107e05241c09a52d804a18982a555fc0def251e05abc9beed7ecad64b38
O=C(OCc1ccccc1)N1CCC2(CO2)C1
[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[C;H0;D3;+0:6](=[CH;D2;+0:7]-[C;D1;H3:8])-[C:9]-[C:10]-1>>[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[C;H0;D4;+0:6]2(-[#8:11]-[CH;D3;+0:7]-2-[C;D1;H3:8])-[C:9]-[C:10]-1
44.8
[{"value": 44.8, "product": "C(C1=CC=CC=C1)OC(=O)N1CC2(C(O2)C)CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3-ethylidenepyrrolidine-1-carboxylic acid benzyl ester (Example A8, 0.65 g, 2.8 mmol) and 3-chloroperoxybenzoic acid (0.86 g, 5 mmol) in dichloromethane (15 mL) is stirred at room temperature for 3 hours. The excess peracid is decomposed by the addition of 10% sodium sulfite. The organic layer is washed w...
10.6084/m9.figshare.5104873.v1
null
null
Ether
C1CC[NH]C1
C1CC2(C[NH]1)CO2
C1CC2(C[NH]1)CO2.c1ccccc1
Other
ClCCl
null
null
CC=C1CCN(C(=O)OCc2ccccc2)C1>ClCCl>CC1OC12CCN(C(=O)OCc1ccccc1)C2
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-25d841ff62cf41b6862babb19ab9536f
CC1OC12CCN(C(=O)OCc1ccccc1)C2.[NH4+]>>CC(N)C1(O)CCN(C(=O)OCc2ccccc2)C1
C(C1=CC=CC=C1)OC(=O)N1CC2(C(O2)C)CC1.[OH-].[NH4+].C(C)(=O)OCC>>C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(O)C(C)N
[CH3:1][CH:2]1[C:4]2([O:5]1)[CH2:6][CH2:7][N:8]([C:9](=[O:10])[O:11][CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[CH2:19]2.[NH4+:3]>>[CH3:1][CH:2]([NH2:3])[C:4]1([OH:5])[CH2:6][CH2:7][N:8]([C:9](=[O:10])[O:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[CH2:19]1
CC1OC12CCN(C(=O)OCc1ccccc1)C2.[NH4+]
CC(N)C1(O)CCN(C(=O)OCc2ccccc2)C1
null
null
CO
Functional Group Addition
OtherReaction
db10b7eb178b687892f63f334d8ed428ad001438c623c5a2f88419bcba1448e4
139012d3a263c64bc0bc696a4ebabf621f4b634824ee35698a4e4d48832c8397
O=C(OCc1ccccc1)N1CCCC1
[#7:1]-[C:2]-[C:3]1(-[C:4])-[O;H0;D2;+0:5]-[CH;D3;+0:6]-1-[C;D1;H3:7].[NH4+;D0:8]>>[#7:1]-[C:2]-[C:3](-[OH;D1;+0:5])(-[CH;D3;+0:6](-[C;D1;H3:7])-[NH2;D1;+0:8])-[C:4]
null
[]
null
null
null
null
A solution of 2-methyl-1-oxa-5-azaspiro[2,4]heptane-5-carboxylic acid benzyl ester (Example A9, 0.31 g, 1.25 mmol) in methanol (10 mL) and ammonium hydroxide (7 mL) is heated in a sealed tube at 100° C. for 16 hours. After cooling, the reaction mixture is dissolved ethyl acetate, washed with water, dried over Na2SO4 an...
10.6084/m9.figshare.5104873.v1
null
Ether
Tertiary alcohol.Primary amine
C1CC2(C[NH]1)CO2
null
C1CC[NH]C1.c1ccccc1
null
CO
null
null
CC1OC12CCN(C(=O)OCc1ccccc1)C2.[NH4+]>CO>CC(N)C1(O)CCN(C(=O)OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-59aeace69c524501960f8f1eb266305a
CC(N)C1(O)CCN(C(=O)OCc2ccccc2)C1.O=Cc1ccccc1O>>CC(N=Cc1ccccc1O)C1(O)CCN(C(=O)OCc2ccccc2)C1
C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(O)C(C)N.C(C=1C(O)=CC=CC1)=O>>C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(C(C)N=CC1=C(C=CC=C1)O)O
[CH3:1][CH:2]([NH2:3])[C:12]1([OH:13])[CH2:14][CH2:15][N:16]([C:17](=[O:18])[O:19][CH2:20][c:21]2[cH:22][cH:23][cH:24][cH:25][cH:26]2)[CH2:27]1.O=[CH:4][c:5]1[cH:6][cH:7][cH:8][cH:9][c:10]1[OH:11]>>[CH3:1][CH:2]([N:3]=[CH:4][c:5]1[cH:6][cH:7][cH:8][cH:9][c:10]1[OH:11])[C:12]1([OH:13])[CH2:14][CH2:15][N:16]([C:17](=[O:1...
CC(N)C1(O)CCN(C(=O)OCc2ccccc2)C1.O=Cc1ccccc1O
CC(N=Cc1ccccc1O)C1(O)CCN(C(=O)OCc2ccccc2)C1
null
null
C(C)O
Heteroatom Alkylation and Arylation
Addition of primary amines to aldehydes/thiocarbonyls
d409dfd3247abb6c1b1364aec380d25720f21e374fd2124063f2d2ce54d31c4f
9b341044a5a058244685b0b956d33f593ccdcd7346fa1d8d7b98a302fd35b8a2
O=C(OCc1ccccc1)N1CCC(CN=Cc2ccccc2)C1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6](-[C;D1;H3:7])-[NH2;D1;+0:8]>>[C:5]-[C:6](-[C;D1;H3:7])-[N;H0;D2;+0:8]=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]
35
[{"value": 35.0, "product": "C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(C(C)N=CC1=C(C=CC=C1)O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3-(1-aminoethyl)-3-hydroxypyrrolidine-1-carboxylic acid benzyl ester (Example A10, 0.34 g, 0.93 mmol) and salicylaldehyde (0.147 g, 1.2 mmol) in dry ethanol (5 mL) is refluxed for 3 hours. After evaporation of the solvent, the residue is purified by column chromatography (30:70:0.01 ethyl acetate/hexanes/...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine
Substituted imine
null
null
c1ccccc1.C1CC[NH]C1.c1ccccc1
HO-
C(C)O
null
null
CC(N)C1(O)CCN(C(=O)OCc2ccccc2)C1.O=Cc1ccccc1O>C(C)O>CC(N=Cc1ccccc1O)C1(O)CCN(C(=O)OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2fa500ca7b4944fca84a3d33e9d249ba
CC(N=[N+]=[N-])C1(F)CCN(C(=O)OCc2ccccc2)C1>>CC(N)C1(F)CCN(C(=O)OCc2ccccc2)C1
C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(F)C(C)N=[N+]=[N-].[H][H]>>C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(F)C(C)N
[N-]=[N+]=[N:3][CH:2]([CH3:1])[C:4]1([F:5])[CH2:6][CH2:7][N:8]([C:9](=[O:10])[O:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[CH2:19]1>>[CH3:1][CH:2]([NH2:3])[C:4]1([F:5])[CH2:6][CH2:7][N:8]([C:9](=[O:10])[O:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[CH2:19]1
CC(N=[N+]=[N-])C1(F)CCN(C(=O)OCc2ccccc2)C1
CC(N)C1(F)CCN(C(=O)OCc2ccccc2)C1
null
[Ni]
CO
Reduction
Azide to amine reduction (Staudinger)
4c9e4990dae2bb965dec06bd45e318560989ee3681b61e443f7aa363b7cfa222
cd009d687d606bf351eac9390a176d16be38f2c8216a599b398641009c215027
O=C(OCc1ccccc1)N1CCCC1
[C:1]-[C:2](-[C;D1;H3:3])-[N;H0;D2;+0:4]=[N+]=[N-]>>[C:1]-[C:2](-[C;D1;H3:3])-[NH2;D1;+0:4]
90.1
[{"value": 90.1, "product": "C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(F)C(C)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3-(1-azidoethyl)-3-fluoropyrrolidine-1-carboxylic acid benzyl ester (Example A16, 0.16 g, 0.5 mmol) in methanol (10 mL) is treated with Raney nickel (100 mg, wet weight) and shaken in a hydrogen atmosphere at room temperature and at 55 psi for 17 hours. The catalyst is removed by filtration through Celite...
10.6084/m9.figshare.5104873.v1
null
Azide
Primary amine
null
null
C1CC[NH]C1.c1ccccc1
Other
[Ni].CO
null
null
CC(N=[N+]=[N-])C1(F)CCN(C(=O)OCc2ccccc2)C1>[Ni].CO>CC(N)C1(F)CCN(C(=O)OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bb473ca2021b44e6ad238522ab891e1c
COCC1(CN2C(=O)c3ccccc3C2=O)CCN(Cc2ccccc2)C1>>COCC1(CN)CCN(Cc2ccccc2)C1
O.NN.C(C1=CC=CC=C1)N1CC(CC1)(COC)CN1C(C2=CC=CC=C2C1=O)=O.Cl>>C(C1=CC=CC=C1)N1CC(CC1)(COC)CN
O=C1c2ccccc2C(=O)[N:6]1[CH2:5][C:4]1([CH2:3][O:2][CH3:1])[CH2:7][CH2:8][N:9]([CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[CH2:17]1>>[CH3:1][O:2][CH2:3][C:4]1([CH2:5][NH2:6])[CH2:7][CH2:8][N:9]([CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[CH2:17]1
COCC1(CN2C(=O)c3ccccc3C2=O)CCN(Cc2ccccc2)C1
COCC1(CN)CCN(Cc2ccccc2)C1
null
null
C(C)O
Reduction
Phthalimide deprotection
d9f63cee80ef758bd939ff2a10772447b3092f1576180488281833a98eb1691a
dbfe4201a9328005dfaec4c3f363ddbb4ef3c9b825f648735dc97b2b57396333
c1ccc(CN2CCCC2)cc1
O=C1-[N;H0;D3;+0:1](-[C:2]-[C:3])-C(=O)-c2:c:c:c:c:c:2-1>>[C:3]-[C:2]-[NH2;D1;+0:1]
89.5
[{"value": 89.5, "product": "C(C1=CC=CC=C1)N1CC(CC1)(COC)CN", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Hydrazine hydrate (85% solution in water, 0.372 g, 6.32 mmol) is added to a solution of 2-(1-benzyl-3-methoxymethylpyrrolidin-3-ylmethyl)isoindole-1,3-dione (Example A20, 1.581 g, 4.34 mmol) in ethanol (50 mL). The resulting mixture is refluxed for 4.5 hours, cooled and acidified with concentrated hydrochloric acid. Th...
10.6084/m9.figshare.5104873.v1
null
Substituted dicarboximide
Primary amine
c1ccc2c(c1)C[NH]C2
null
C1CC[NH]C1.c1ccccc1
HO-
C(C)O
null
null
COCC1(CN2C(=O)c3ccccc3C2=O)CCN(Cc2ccccc2)C1>C(C)O>COCC1(CN)CCN(Cc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-99e603ae99de436a99dec9c803eff8bd
CC1OC12CCN(C(=O)OCc1ccccc1)C2.F>>CC(O)C1(F)CCN(C(=O)OCc2ccccc2)C1
C(C1=CC=CC=C1)OC(=O)N1CC2(C(O2)C)CC1.N1=CC=CC=C1.F>>C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(C(C)O)F
[CH3:1][CH:2]1[O:3][C:4]12[CH2:6][CH2:7][N:8]([C:9](=[O:10])[O:11][CH2:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1)[CH2:19]2.[FH:5]>>[CH3:1][CH:2]([OH:3])[C:4]1([F:5])[CH2:6][CH2:7][N:8]([C:9](=[O:10])[O:11][CH2:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)[CH2:19]1
CC1OC12CCN(C(=O)OCc1ccccc1)C2.F
CC(O)C1(F)CCN(C(=O)OCc2ccccc2)C1
null
null
ClCCl
Miscellaneous
OtherReaction
104f13bbcfd8fe847bc8f50c2882a7ad8914446786de7a041173f811193dc35d
3308376c1af9182795876175318589d58f2494c98ab8c1da1abbbdb180da2297
O=C(OCc1ccccc1)N1CCCC1
[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[C;H0;D4;+0:6]2(-[C:7]-[C:8]-1)-[O;H0;D2;+0:9]-[C:10]-2-[C;D1;H3:11].[FH;D0;+0:12]>>[#8:1]-[C:2](=[O;D1;H0:3])-[#7:4]1-[C:5]-[C;H0;D4;+0:6](-[F;H0;D1;+0:12])(-[C:10](-[C;D1;H3:11])-[OH;D1;+0:9])-[C:7]-[C:8]-1
null
[]
null
null
3
HOUR
A solution of 0.247 g, (1 mmol) of 2-methyl-1-oxa-5-azaspiro[2,4]-heptane-5-carboxylic acid benzyl ester (Example A9) in dichloromethane (3 mL) is added to a polypropylene flask containing 0.5 mL of hydrogen fluoride-pyridine at −40° C. The reaction is allowed to come to room temperature and stirring is continued for 3...
10.6084/m9.figshare.5104873.v1
null
Ether
Tertiary halide.Secondary alcohol
C1CC2(C[NH]1)CO2
C1CC[NH]C1
C1CC[NH]C1.c1ccccc1
null
ClCCl
null
3
CC1OC12CCN(C(=O)OCc1ccccc1)C2.F>ClCCl>CC(O)C1(F)CCN(C(=O)OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f78574fb405d489d91af7e5ae9751dd2
CC(O)C1(F)CCN(C(=O)OCc2ccccc2)C1.CS(=O)(=O)Cl>>CC(OS(C)(=O)=O)C1(F)CCN(C(=O)OCc2ccccc2)C1
C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(C(C)O)F.C(C)N(CC)CC.CS(=O)(=O)Cl>>C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(C(C)OS(=O)(=O)C)F
[CH3:1][CH:2]([OH:3])[C:8]1([F:9])[CH2:10][CH2:11][N:12]([C:13](=[O:14])[O:15][CH2:16][c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[CH2:23]1.Cl[S:4]([CH3:5])(=[O:6])=[O:7]>>[CH3:1][CH:2]([O:3][S:4]([CH3:5])(=[O:6])=[O:7])[C:8]1([F:9])[CH2:10][CH2:11][N:12]([C:13](=[O:14])[O:15][CH2:16][c:17]2[cH:18][cH:19][cH:20][cH:21]...
CC(O)C1(F)CCN(C(=O)OCc2ccccc2)C1.CS(=O)(=O)Cl
CC(OS(C)(=O)=O)C1(F)CCN(C(=O)OCc2ccccc2)C1
null
null
ClCCl
Acylation
Formation of Sulfonic Esters
641955d0081c80f158ce2aacd31873a3f3301c87ca0800cf263e288ba8390217
4f9373df8a11470603daf885a5777cebf95940370e32739263d35df0f171a0dd
O=C(OCc1ccccc1)N1CCCC1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[C:5]-[C:6](-[C;D1;H3:7])-[OH;D1;+0:8]>>[C:5]-[C:6](-[C;D1;H3:7])-[O;H0;D2;+0:8]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
95.5
[{"value": 95.5, "product": "C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(C(C)OS(=O)(=O)C)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a −10° C. solution of 3-fluoro-3-(1-hydroxyethyl)pyrrolidine-1-carboxylic acid benzyl ester (Example A14, 0.267 g, 1.00 mmol), triethylamine (0.4 g, 4 mmol) and dichloromethane (10 mL) is added methanesulfonyl chloride (0.229 g, 2.00 mmol). The mixture is stirred at room temperature for 2 hours and concentrated in v...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Sulfonyl halide
Mesylate
null
null
C1CC[NH]C1.c1ccccc1
HCl
ClCCl
null
2
CC(O)C1(F)CCN(C(=O)OCc2ccccc2)C1.CS(=O)(=O)Cl>ClCCl>CC(OS(C)(=O)=O)C1(F)CCN(C(=O)OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-28a8f740c3c44d56886c2f08e9774695
CC(OS(C)(=O)=O)C1(F)CCN(C(=O)OCc2ccccc2)C1.[N-]=[N+]=[N-]>>CC(N=[N+]=[N-])C1(F)CCN(C(=O)OCc2ccccc2)C1
C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(C(C)OS(=O)(=O)C)F.[N-]=[N+]=[N-].[Na+]>>C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(F)C(C)N=[N+]=[N-]
CS(=O)(=O)O[CH:2]([CH3:1])[C:6]1([F:7])[CH2:8][CH2:9][N:10]([C:11](=[O:12])[O:13][CH2:14][c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[CH2:21]1.[N-:3]=[N+:4]=[N-:5]>>[CH3:1][CH:2]([N:3]=[N+:4]=[N-:5])[C:6]1([F:7])[CH2:8][CH2:9][N:10]([C:11](=[O:12])[O:13][CH2:14][c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[CH2:21]1
CC(OS(C)(=O)=O)C1(F)CCN(C(=O)OCc2ccccc2)C1.[N-]=[N+]=[N-]
CC(N=[N+]=[N-])C1(F)CCN(C(=O)OCc2ccccc2)C1
null
null
O.CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
341eb24906c58cd9cfdeec13febaf0724780d7854e6b6d7ec703218c4bcbe27b
5f2cb2b9819a73a6855f5277f7fe9d5ce3871340baaebb59d42e38e1ca145c0a
O=C(OCc1ccccc1)N1CCCC1
C-S(=O)(=O)-O-[CH;D3;+0:1](-[C;D1;H3:2])-[C:3](-[F;D1;H0:4])(-[C:5])-[C:6]-[#7:7].[N-;H0;D1:8]=[#7;+:9]=[N;-;D1;H0:10]>>[#7:7]-[C:6]-[C:3](-[F;D1;H0:4])(-[CH;D3;+0:1](-[C;D1;H3:2])-[N;H0;D2;+0:8]=[#7;+:9]=[N;-;D1;H0:10])-[C:5]
76
[{"value": 76.0, "product": "C(C1=CC=CC=C1)OC(=O)N1CC(CC1)(F)C(C)N=[N+]=[N-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
120
CELSIUS
null
null
To a solution of 3-fluoro-3-(1-methanesulfonyloxyethyl)pyrrolidine-1-carboxylic acid benzyl ester (Example A15, 0.25 g, 0.72 mmol) in N,N-dimethylformamide (5 mL) is added sodium azide (0.13 g, 2 mmol). The reaction mixture is heated at 120° C. overnight. The mixture is diluted with water and extracted with ethyl aceta...
10.6084/m9.figshare.5104873.v1
null
Mesylate
Azide
null
null
C1CC[NH]C1.c1ccccc1
MsOH.HO-
O.CN(C=O)C
120
null
CC(OS(C)(=O)=O)C1(F)CCN(C(=O)OCc2ccccc2)C1.[N-]=[N+]=[N-]>O.CN(C=O)C>CC(N=[N+]=[N-])C1(F)CCN(C(=O)OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bda05e49b0404071a41e804aec975155
C=C(CBr)C(=O)OCC.C[O-]>>C=C(COC)C(=O)OCC
BrCC(C(=O)OCC)=C.C[O-].[Na+]>>C(C)OC(C(=C)COC)=O
Br[CH2:3][C:2](=[CH2:1])[C:6](=[O:7])[O:8][CH2:9][CH3:10].[O-:4][CH3:5]>>[CH2:1]=[C:2]([CH2:3][O:4][CH3:5])[C:6](=[O:7])[O:8][CH2:9][CH3:10]
C=C(CBr)C(=O)OCC.C[O-]
C=C(COC)C(=O)OCC
null
null
CO.O
Heteroatom Alkylation and Arylation
OtherReaction
3dd6ea90858eede84ece2f60931b760bd509d5f421f2feb2b0fe7a2c006d84f0
62c7c72c35b09d63ca1131e6cd8c0b88a31e29901d660456b77319cfd78354c7
null
Br-[CH2;D2;+0:1]-[C:2](=[C;D1;H2:3])-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7].[C;D1;H3:8]-[O-;H0;D1:9]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[C:2](=[C;D1;H2:3])-[CH2;D2;+0:1]-[O;H0;D2;+0:9]-[C;D1;H3:8]
28.7
[{"value": 28.7, "product": "C(C)OC(C(=C)COC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of ethyl α-(bromomethyl)acrylate (0.99 g, 5.1 mmol [Villieras J., Rambaud M., Synthesis, 1982:924–926]) in methanol (10 mL) is added to an ice-cold solution of sodium methoxide (0.33 g, 6.1 mmol) in methanol (50 mL). The suspension is refluxed for 21 hours, cooled, diluted with water and extracted with dichl...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Ether
null
null
null
Br-
CO.O
null
null
C=C(CBr)C(=O)OCC.C[O-]>CO.O>C=C(COC)C(=O)OCC
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e346e5323871419b8510bb1982209d01
CCOC(=O)C1(COC)CCN(Cc2ccccc2)C1>>COCC1(CO)CCN(Cc2ccccc2)C1
C(C)OC(=O)C1(CN(CC1)CC1=CC=CC=C1)COC.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>C(C1=CC=CC=C1)N1CC(CC1)(COC)CO
CCO[C:5]([C:4]1([CH2:3][O:2][CH3:1])[CH2:7][CH2:8][N:9]([CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[CH2:17]1)=[O:6]>>[CH3:1][O:2][CH2:3][C:4]1([CH2:5][OH:6])[CH2:7][CH2:8][N:9]([CH2:10][c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[CH2:17]1
CCOC(=O)C1(COC)CCN(Cc2ccccc2)C1
COCC1(CO)CCN(Cc2ccccc2)C1
null
null
O1CCCC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(CN2CCCC2)cc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3](-[C:4])(-[C:5])-[C:6]-[#7:7]>>[#7:7]-[C:6]-[C:3](-[C:4])(-[CH2;D2;+0:1]-[OH;D1;+0:2])-[C:5]
87.5
[{"value": 87.5, "product": "C(C1=CC=CC=C1)N1CC(CC1)(COC)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of 1-benzyl-3-methoxymethylpyrrolidine-3-carboxylic acid ethyl ester (Example A18a, 2.30 g, 8.3 mmol) in anhydrous tetrahydrofuran (10 mL) is added dropwise to an ice-cold suspension of lithium aluminum hydride (0.821 g, 22 mmol) in tetrahydrofuran (50 mL). The resulting mixture is stirred at room temperatur...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
C1CC[NH]C1.c1ccccc1
HO-
O1CCCC1
null
18
CCOC(=O)C1(COC)CCN(Cc2ccccc2)C1>O1CCCC1>COCC1(CO)CCN(Cc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7817712f962644f282f5a64037189394
COCC1(CO)CCN(Cc2ccccc2)C1.O=C1NC(=O)c2ccccc21>>COCC1(CN2C(=O)c3ccccc3C2=O)CCN(Cc2ccccc2)C1
N(=NC(=O)OCC)C(=O)OCC.C(C1=CC=CC=C1)N1CC(CC1)(COC)CO.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(C=2C(C(N1)=O)=CC=CC2)=O>>C(C1=CC=CC=C1)N1CC(CC1)(COC)CN1C(C2=CC=CC=C2C1=O)=O
O[CH2:5][C:4]1([CH2:3][O:2][CH3:1])[CH2:17][CH2:18][N:19]([CH2:20][c:21]2[cH:22][cH:23][cH:24][cH:25][cH:26]2)[CH2:27]1.[NH:6]1[C:7](=[O:8])[c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]2[C:15]1=[O:16]>>[CH3:1][O:2][CH2:3][C:4]1([CH2:5][N:6]2[C:7](=[O:8])[c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[C:15]2=[O:16])[CH2:17][CH2:18...
COCC1(CO)CCN(Cc2ccccc2)C1.O=C1NC(=O)c2ccccc21
COCC1(CN2C(=O)c3ccccc3C2=O)CCN(Cc2ccccc2)C1
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
Mitsunobu_imide
16aabf490ad1bd0cd53a985dff922c76188147a3ad5bf7d09c4c1e93a9e46a19
8a66434962da2945c8a8685e3bd4f60c7955241df224c95aa14ead6db9d240f9
O=C1c2ccccc2C(=O)N1CC1CCN(Cc2ccccc2)C1
O-[CH2;D2;+0:1]-[C:2](-[C:3])(-[C:4])-[C:5]-[#7:6].[O;D1;H0:7]=[C:8]1-[NH;D2;+0:9]-[C:10](=[O;D1;H0:11])-[c:12]:[c:13]-1>>[#7:6]-[C:5]-[C:2](-[C:3])(-[CH2;D2;+0:1]-[N;H0;D3;+0:9]1-[C:8](=[O;D1;H0:7])-[c:13]:[c:12]-[C:10]-1=[O;D1;H0:11])-[C:4]
21.9
[{"value": 21.9, "product": "C(C1=CC=CC=C1)N1CC(CC1)(COC)CN1C(C2=CC=CC=C2C1=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of (1-benzyl-3-methoxymethylpyrrolidin-3-yl)methanol (Example A19, 1.71 g, 7.27 mmol), triphenylphosphine (2.16 g, 8.22 mmol), phthalimide (1.14 g, 7.73 mmol), and anhydrous tetrahydrofuran is cooled to 0° C. and treated with diethyl azodicarboxylate (1.62 g, 9.31 mmol). The resulting mixture is stirred at r...
10.6084/m9.figshare.5104873.v1
null
Unsubstituted dicarboximide.Primary alcohol
Substituted dicarboximide
c1ccc2c(c1)CNC2
c1ccc2c(c1)C[NH]C2
c1ccc2c(c1)C[NH]C2.C1CC[NH]C1.c1ccccc1
HO-
O1CCCC1
null
18
COCC1(CO)CCN(Cc2ccccc2)C1.O=C1NC(=O)c2ccccc21>O1CCCC1>COCC1(CN2C(=O)c3ccccc3C2=O)CCN(Cc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d2eb413225c145a683f8e6c5e0750cba
BrCc1ccccc1.O=C(O)C1CCCNC1>>O=C(OCc1ccccc1)C1CCCN(Cc2ccccc2)C1
N1CC(C(=O)O)CCC1.C(C1=CC=CC=C1)Br.C([O-])([O-])=O.[K+].[K+]>>C(C1=CC=CC=C1)OC(=O)C1CN(CCC1)CC1=CC=CC=C1
Br[CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1.[O:1]=[C:2]([OH:3])[CH:11]1[CH2:12][CH2:13][CH2:14][NH:15][CH2:23]1>>[O:1]=[C:2]([O:3][CH2:4][c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[CH:11]1[CH2:12][CH2:13][CH2:14][N:15]([CH2:16][c:17]2[cH:18][cH:19][cH:20][cH:21][cH:22]2)[CH2:23]1
BrCc1ccccc1.O=C(O)C1CCCNC1
O=C(OCc1ccccc1)C1CCCN(Cc2ccccc2)C1
null
null
C(C)(=O)OCC.O.CN(C=O)C
Aromatic Heterocycle Formation
OtherReaction
5ae533ced5e169e93e6b08a630ab609c527b470a1c1cbce279f0db2c2352f95a
2fa0f0da58593fdbf30a4a755d6a9f73d3447f670f3350f46ceac20cd57d879f
O=C(OCc1ccccc1)C1CCCN(Cc2ccccc2)C1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]-[C:10](=[O;D1;H0:11])-[OH;D1;+0:12]>>[C:5]-[C:6]-[N;H0;D3;+0:7](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:8]-[C:9]-[C:10](=[O;D1;H0:11])-[O;H0;D2;+0:12]-[C:13]-[c:14]
44.9
[{"value": 44.9, "product": "C(C1=CC=CC=C1)OC(=O)C1CN(CCC1)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
null
null
To a solution added of nipecotic acid (8.0 g, 61.9 mmol) in N,N-dimethylformamide (80 mL) is benzyl bromide (31.8 g, 186 mmol) and potassium carbonate (42.8 g, 310 mmol). The mixture is heated at 70° C. for 18 hours and diluted with ethyl acetate and water. The organic extract is washed with 1.0 M hydrochloric acid, wa...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carboxylic acid.Secondary amine
Ester.Tertiary amine
C1CCNCC1
c1ccccc1.C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1.c1ccccc1
Br-
C(C)(=O)OCC.O.CN(C=O)C
70
null
BrCc1ccccc1.O=C(O)C1CCCNC1>C(C)(=O)OCC.O.CN(C=O)C>O=C(OCc1ccccc1)C1CCCN(Cc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-97eef82bec22448db417033565e432c7
O=C(OCc1ccccc1)C1CCCN(Cc2ccccc2)C1>>O=C(O)C1CCCN(Cc2ccccc2)C1
C(C1=CC=CC=C1)OC(=O)C1CN(CCC1)CC1=CC=CC=C1.[OH-].[Na+]>>C(C1=CC=CC=C1)N1CC(CCC1)C(=O)O
c1ccc(C[O:3][C:2](=[O:1])[CH:4]2[CH2:5][CH2:6][CH2:7][N:8]([CH2:9][c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[CH2:16]2)cc1>>[O:1]=[C:2]([OH:3])[CH:4]1[CH2:5][CH2:6][CH2:7][N:8]([CH2:9][c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)[CH2:16]1
O=C(OCc1ccccc1)C1CCCN(Cc2ccccc2)C1
O=C(O)C1CCCN(Cc2ccccc2)C1
null
null
CO
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(CN2CCCCC2)cc1
[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]
94
[{"value": 94.0, "product": "C(C1=CC=CC=C1)N1CC(CCC1)C(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
To a solution 3.0 g (9.7 mmol) of 1-benzylpiperidine-3-carboxylic acid benzyl ester (Example A21) in methanol (20 mL) was added 1N sodium hydroxide (20 mL), and the reaction is stirred at room temperature for 18 hours. The methanol is removed in vacuo and the basic aqueous solution is acidified to pH 4 with 1.0 M hydro...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
C1CC[NH]CC1.c1ccccc1
Other
CO
null
18
O=C(OCc1ccccc1)C1CCCN(Cc2ccccc2)C1>CO>O=C(O)C1CCCN(Cc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-043784f2e57d4bdc9a6caa9b5a21c527
CC(C)(C)OC(=O)N1CCC2CN(Cc3ccccc3)CC2C1>>CC(C)(C)OC(=O)N1CCC2CNCC2C1
C(C)(C)(C)OC(=O)N1CC2C(CC1)CN(C2)CC2=CC=CC=C2.[H][H]>>C(C)(C)(C)OC(=O)N1CC2C(CC1)CNC2
c1ccc(C[N:13]2[CH2:12][CH:11]3[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:16][CH:15]3[CH2:14]2)cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]2[CH2:12][NH:13][CH2:14][CH:15]2[CH2:16]1
CC(C)(C)OC(=O)N1CCC2CN(Cc3ccccc3)CC2C1
CC(C)(C)OC(=O)N1CCC2CNCC2C1
null
[Pd]
CO
Deprotection
Hydrogenolysis of tertiary amines
9251f3ece1810ac4ff2e2dcb7d0b77a547db13ef1851b4999cec798870900a19
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
C1CC2CNCC2CN1
C(-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1)-c1:c:c:c:c:c:1>>[C:3]1-[C:2]-[NH;D2;+0:1]-[C:5]-[C:4]-1
99.8
[{"value": 99.8, "product": "C(C)(C)(C)OC(=O)N1CC2C(CC1)CNC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Benzyloctahydropyrrolo[3,4-c]pyridine-5-carboxylic acid tert-butyl ester (Example A26, 24.98 g, 78.8 mmol) in 400 mL of methanol is treated with 2.5 g of 20% Pd/C and shaken for 20.5 hours under 50 PSI of hydrogen. The solution is filtered and concentrated to afford 17.8 g of the title compound as a solid. MS APCI: m...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.C1CC2C[NH]CC2C[NH]1
C1CC2CNCC2C[NH]1
C1CC2CNCC2C[NH]1
Other
[Pd].CO
null
null
CC(C)(C)OC(=O)N1CCC2CN(Cc3ccccc3)CC2C1>[Pd].CO>CC(C)(C)OC(=O)N1CCC2CNCC2C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a9a5e5f0de004235805830ca3e08b53b
CCOC(=O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1>>O=C(O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1
C(C)OC(=O)C1(CN(CC1)CC1=CC=CC=C1)CC1=CC=CC=C1.[OH-].[Na+]>>C(C1=CC=CC=C1)N1CC(CC1)(C(=O)O)CC1=CC=CC=C1
CC[O:3][C:2](=[O:1])[C:4]1([CH2:5][c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[CH2:12][CH2:13][N:14]([CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:22]1>>[O:1]=[C:2]([OH:3])[C:4]1([CH2:5][c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[CH2:12][CH2:13][N:14]([CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:22]1
CCOC(=O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1
O=C(O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1
null
null
CO
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(CC2CCN(Cc3ccccc3)C2)cc1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
76.8
[{"value": 76.8, "product": "C(C1=CC=CC=C1)N1CC(CC1)(C(=O)O)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 1,3-dibenzylpyrrolidine-3-carboxylic acid ethyl ester (Example A18e, 13.1 g, 41 mmol) in 250 mL of methanol is added 2N NaOH (46 mL, 92 mmol) and the reaction is heated to reflux for 24 hours. The solution is cooled, concentrated, redissolved in water and extracted with ether. The pH of the aqueous lay...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.C1CC[NH]C1.c1ccccc1
Other
CO
null
null
CCOC(=O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1>CO>O=C(O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-02ad2852ead94e6593b17d452a0bcb4b
O=C(O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1.[NH4+]>>NC(=O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1
[NH4+].[OH-].C(C1=CC=CC=C1)N1CC(CC1)(C(=O)O)CC1=CC=CC=C1.C(=O)(N1C=NC=C1)N1C=NC=C1.C(C)N(CC)CC>>C(C1=CC=CC=C1)N1CC(CC1)(C(=O)N)CC1=CC=CC=C1
O[C:2](=[O:3])[C:4]1([CH2:5][c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[CH2:12][CH2:13][N:14]([CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:22]1.[NH4+:1]>>[NH2:1][C:2](=[O:3])[C:4]1([CH2:5][c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[CH2:12][CH2:13][N:14]([CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:22]...
O=C(O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1.[NH4+]
NC(=O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1
null
null
O1CCCC1
Acylation
Carboxylic acid to amide conversion
1283aef55d7ee699f097a8e5267689198c76ba671644401547f902657820236d
cb0a71c3fb37a76e96fbd81aae6f95a28398a03d1ad2c8e877085e735efb98f1
c1ccc(CC2CCN(Cc3ccccc3)C2)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])(-[C:5])-[C:6]-[#7:7].[NH4+;D0:8]>>[#7:7]-[C:6]-[C:3](-[C:4])(-[C;H0;D3;+0:1](-[NH2;D1;+0:8])=[O;D1;H0:2])-[C:5]
103.9
[{"value": 103.9, "product": "C(C1=CC=CC=C1)N1CC(CC1)(C(=O)N)CC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A mixture of 1,3-dibenzylpyrrolidine-3-carboxylic acid (Example A28, 4.0 g, 13.5 mmol), 1,1′-carbonyldiimidazole (2.42 g, 14.9 mmol), and triethylamine (2.08 mL, 14.9 mmol) in tetrahydrofuran (100 mL) is heated at reflux for 1.5 hours. The solution is cooled, poured into NH4OH (300 mL), and stirred for 18 hours. The mi...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary amide
null
null
c1ccccc1.C1CC[NH]C1.c1ccccc1
HO-
O1CCCC1
null
18
O=C(O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1.[NH4+]>O1CCCC1>NC(=O)C1(Cc2ccccc2)CCN(Cc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-07031ad2da014fb091396545797a8366
CC(C)(C)OC(=O)NC1(c2ccccc2)CCN(Cc2ccccc2)C1>>CC(C)(C)OC(=O)NC1(c2ccccc2)CCNC1
C(C)(C)(C)OC(NC1(CN(CC1)CC1=CC=CC=C1)C1=CC=CC=C1)=O.[H][H]>>C(C)(C)(C)OC(NC1(CNCC1)C1=CC=CC=C1)=O
c1ccc(C[N:18]2[CH2:17][CH2:16][C:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])([c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[CH2:19]2)cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C:9]1([c:10]2[cH:11][cH:12][cH:13][cH:14][cH:15]2)[CH2:16][CH2:17][NH:18][CH2:19]1
CC(C)(C)OC(=O)NC1(c2ccccc2)CCN(Cc2ccccc2)C1
CC(C)(C)OC(=O)NC1(c2ccccc2)CCNC1
null
[Pd]
CO
Deprotection
Hydrogenolysis of tertiary amines
846a35f8c83fa58d2c714915319a8bc96745602a4dd9ac20dbad14bc1e16a470
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
c1ccc(C2CCNC2)cc1
C(-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1)-c1:c:c:c:c:c:1>>[C:3]1-[C:2]-[NH;D2;+0:1]-[C:5]-[C:4]-1
99.9
[{"value": 99.9, "product": "C(C)(C)(C)OC(NC1(CNCC1)C1=CC=CC=C1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
(1-Benzyl-3-phenylpyrrolidin-3-yl)carbamic acid tert-butyl ester (Hagen S. E., Domagala J. M., Heifetz C. L., Sanchez J. P., Solomon M., J. Med. Chem., 1990; 33(2):849–854) (2.79 g, 7.9 mmol) in 100 mL of methanol is treated with 1.0 g of 20% Pd/C and shaken for 17 hours under 50 psi of hydrogen. The solution is filter...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.C1CC[NH]C1
C1CCNC1
c1ccccc1.C1CCNC1
Other
[Pd].CO
null
null
CC(C)(C)OC(=O)NC1(c2ccccc2)CCN(Cc2ccccc2)C1>[Pd].CO>CC(C)(C)OC(=O)NC1(c2ccccc2)CCNC1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4019104aa7ff436fb7ae8cac196a3a8a
CCc1ccc(Cc2c[nH]c3ccc([C@@H]4O[C@H](COCc5ccccc5)[C@@H](OCc5ccccc5)[C@H](OCc5ccccc5)[C@H]4OCc4ccccc4)cc23)cc1>>CCc1ccc(Cc2c[nH]c3ccc([C@@H]4O[C@H](CO)[C@@H](O)[C@H](O)[C@H]4O)cc23)cc1
C(C)C1=CC=C(CC2=CNC3=CC=C(C=C23)[C@H]2[C@H](OCC3=CC=CC=C3)[C@@H](OCC3=CC=CC=C3)[C@H](OCC3=CC=CC=C3)[C@H](O2)COCC2=CC=CC=C2)C=C1.[OH-].[Na+]>>C(C)C1=CC=C(CC2=CNC3=CC=C(C=C23)[C@H]2[C@H](O)[C@@H](O)[C@H](O)[C@H](O2)CO)C=C1
c1ccc(C[O:19][CH2:18][C@H:17]2[O:16][C@@H:15]([c:14]3[cH:13][cH:12][c:11]4[nH:10][cH:9][c:8]([CH2:7][c:6]5[cH:5][cH:4][c:3]([CH2:2][CH3:1])[cH:29][cH:28]5)[c:27]4[cH:26]3)[C@H:24]([O:25]Cc3ccccc3)[C@@H:22]([O:23]Cc3ccccc3)[C@@H:20]2[O:21]Cc2ccccc2)cc1>>[CH3:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][c:8]2[cH:9][nH:10][c:...
CCc1ccc(Cc2c[nH]c3ccc([C@@H]4O[C@H](COCc5ccccc5)[C@@H](OCc5ccccc5)[C@H](OCc5ccccc5)[C@H]4OCc4ccccc4)cc23)cc1
CCc1ccc(Cc2c[nH]c3ccc([C@@H]4O[C@H](CO)[C@@H](O)[C@H](O)[C@H]4O)cc23)cc1
null
null
C1CCOC1.O
Deprotection
OtherReaction
9622096468e29231a13a0af4bb02cbbbed6ada9c44b575de6d474da0d432309d
73dfd818b2d879aa8bc6aaeea5cb523f7f4f5ff62317dd7cb2c99f1b31ec455c
c1ccc(Cc2c[nH]c3ccc([C@H]4CCCCO4)cc23)cc1
C(-[O;H0;D2;+0:1]-[C:2]-[C:3]1-[#8:4]-[C:5]-[C:6](-[O;H0;D2;+0:7]-C-c2:c:c:c:c:c:2)-[C:8](-[O;H0;D2;+0:9]-C-c2:c:c:c:c:c:2)-[C:10]-1-[O;H0;D2;+0:11]-C-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1>>[OH;D1;+0:1]-[C:2]-[C:3]1-[#8:4]-[C:5]-[C:6](-[OH;D1;+0:7])-[C:8](-[OH;D1;+0:9])-[C:10]-1-[OH;D1;+0:11]
85
[{"value": 85.0, "product": "C(C)C1=CC=C(CC2=CNC3=CC=C(C=C23)[C@H]2[C@H](O)[C@@H](O)[C@H](O)[C@H](O2)CO)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
3-(4-Ethylbenzyl)-5-(2,3,4,6-tetra-O-benzyl-β-D-glucopyranosyl)-1H-indole: Part E (0.68 g, 0.78 mmol) was dissolved in THF (15 mL) and 25% aqueous sodium hydroxide (5 mL) and the resulting solution was brought to reflux for 3 h. After cooling to room temperature, the mixture was diluted with water (30 mL), and extracte...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Ether
Primary alcohol.Secondary alcohol.Secondary alcohol.Secondary alcohol
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
null
c1ccccc1.c1ccc2[nH]ccc2c1.C1CCOCC1
Other
C1CCOC1.O
null
null
CCc1ccc(Cc2c[nH]c3ccc([C@@H]4O[C@H](COCc5ccccc5)[C@@H](OCc5ccccc5)[C@H](OCc5ccccc5)[C@H]4OCc4ccccc4)cc23)cc1>C1CCOC1.O>CCc1ccc(Cc2c[nH]c3ccc([C@@H]4O[C@H](CO)[C@@H](O)[C@H](O)[C@H]4O)cc23)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0e53689819a44ea5b6020ddf049fe8f2
CCN.NC(=O)CC[C@H](N)C(=O)O>>CCNC(=O)CC[C@H](N)C(=O)O
N[C@@H](CCC(N)=O)C(=O)O.C(C)N>>N[C@@H](CCC(=O)NCC)C(=O)O
[CH3:1][CH2:2][NH2:3].N[C:4](=[O:5])[CH2:6][CH2:7][C@H:8]([NH2:9])[C:10](=[O:11])[OH:12]>>[CH3:1][CH2:2][NH:3][C:4](=[O:5])[CH2:6][CH2:7][C@H:8]([NH2:9])[C:10](=[O:11])[OH:12]
CCN.NC(=O)CC[C@H](N)C(=O)O
CCNC(=O)CC[C@H](N)C(=O)O
null
null
B([O-])([O-])[O-]
Acylation
OtherReaction
e6b65aa2cf0415dec90d7472d3f0bc6b9ee4b3e1f07ac8a90a77f65444307f4a
cbe2f1d5a907138095943f49f081313fbf3c1706d27fd317bb9c4ee07b790834
null
N-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C;D1;H3:5]-[C:6]-[NH2;D1;+0:7]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:7]-[C:6]-[C;D1;H3:5]
null
[]
null
null
null
null
0.3 M glutamine and 1.5 M ethylamine were allowed to react at 30° C. for 22 hours in borate buffer (Na2B4O7—NaOH, pH 11) in the presence of 0.3 U glutaminase, to give 225 nmol of L-theanine. In addition, a by-product glutamic acid was 20 nmol. The purification of theanine from the reaction mixture was carried out by su...
10.6084/m9.figshare.5104873.v1
null
Primary amide.Primary amine
Secondary amide
null
null
null
Other
B([O-])([O-])[O-]
null
null
CCN.NC(=O)CC[C@H](N)C(=O)O>B([O-])([O-])[O-]>CCNC(=O)CC[C@H](N)C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-15d92f3715f741f0bf46d9dec45f38a3
O=C(O)C1(O)c2ccccc2-c2ccccc21>>COC(=O)C1(O)c2ccccc2-c2ccccc21
OC1(C2=CC=CC=C2C=2C=CC=CC12)C(=O)O.S(O)(O)(=O)=O.C(O)([O-])=O.[Na+]>>OC1(C2=CC=CC=C2C=2C=CC=CC12)C(=O)OC
[OH:2][C:3](=[O:4])[C:5]1([OH:6])[c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2-[c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]21>>[CH3:1][O:2][C:3](=[O:4])[C:5]1([OH:6])[c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2-[c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]21
O=C(O)C1(O)c2ccccc2-c2ccccc21
COC(=O)C1(O)c2ccccc2-c2ccccc21
null
null
CO
Miscellaneous
Protection of carboxylic acid
56520e0abb4535dce9a663824ca803b71c2c0dd72dfd246317d953596a987bd2
2ccc7a30191c2c171b49e8a0217bee87430687dd0f567141eca025a75b7e3136
c1ccc2c(c1)Cc1ccccc1-2
[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]>>[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-[C;D1;H3:5]
null
[]
null
null
null
null
50.4 g (0.223 mol) 9-hydroxy-9-fluorenecarboxylic acid are dissolved in 500 ml of methanol, combined with 5 ml (0.089 mol) conc. sulphuric acid and refluxed for 1 hour. After cooling 100 ml sodium hydrogen carbonate solution (about pH 8) are added, and the methanol is largely distilled off under reduced pressure. The r...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ester
null
null
c1ccc2c(c1)Cc1ccccc12
Other
CO
null
null
O=C(O)C1(O)c2ccccc2-c2ccccc21>CO>COC(=O)C1(O)c2ccccc2-c2ccccc21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ad6c840f68ba450a9407247c4d813150
COC(=O)CC(Br)C=O.Cc1c(Cl)cccc1S(=O)(=O)NC(N)=S>>COC(=O)Cc1cnc(NS(=O)(=O)c2cccc(Cl)c2C)s1
NC(=S)NS(=O)(=O)C1=C(C(=CC=C1)Cl)C.BrC(CC(=O)OC)C=O>>ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)OC)C
O=[CH:7][CH:6](Br)[CH2:5][C:3]([O:2][CH3:1])=[O:4].[NH2:8][C:9]([NH:10][S:11](=[O:12])(=[O:13])[c:14]1[cH:15][cH:16][cH:17][c:18]([Cl:19])[c:20]1[CH3:21])=[S:22]>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][c:6]1[cH:7][n:8][c:9]([NH:10][S:11](=[O:12])(=[O:13])[c:14]2[cH:15][cH:16][cH:17][c:18]([Cl:19])[c:20]2[CH3:21])[s:22]1
COC(=O)CC(Br)C=O.Cc1c(Cl)cccc1S(=O)(=O)NC(N)=S
COC(=O)Cc1cnc(NS(=O)(=O)c2cccc(Cl)c2C)s1
null
null
N1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
1e98d56449369ed49a01def2ba436800fc8285b6f16adfb3ff0f1aaf7f34bbac
1467150cea192c09dd35541b6f6ddef57af2b0cb933fc1eb5dedd0a587a7e1db
O=S(=O)(Nc1nccs1)c1ccccc1
Br-[CH;D3;+0:1](-[C:2]-[C:3](=[O;D1;H0:4])-[#8:5]-[C;D1;H3:6])-[CH;D2;+0:7]=O.[#16:8]-[#7:9]-[C;H0;D3;+0:10](-[NH2;D1;+0:11])=[S;H0;D1;+0:12]>>[#16:8]-[#7:9]-[c;H0;D3;+0:10]1:[n;H0;D2;+0:11]:[cH;D2;+0:7]:[c;H0;D3;+0:1](-[C:2]-[C:3](=[O;D1;H0:4])-[#8:5]-[C;D1;H3:6]):[s;H0;D2;+0:12]:1
null
[]
null
null
null
null
N-(aminocarbonothioyl)-3-chloro-2-methylbenzenesulfonamide (0.4 g, 1.5 mmol) and methyl 3-bromo-4-oxobutanoate (0.3 g, 1.5 mmol), dissolved in pyridine (5 mL), were irradiated in a microwave oven for 2.5 min at 130° C. The solvent was removed under reduced pressure and the product separated from the starting materials ...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Aldehyde.Thiourea
null
null
c1cscn1
c1cscn1.c1ccccc1
HBr
N1=CC=CC=C1
null
null
COC(=O)CC(Br)C=O.Cc1c(Cl)cccc1S(=O)(=O)NC(N)=S>N1=CC=CC=C1>COC(=O)Cc1cnc(NS(=O)(=O)c2cccc(Cl)c2C)s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-83947141fcc74f808a1a2bc552757fcf
COC(=O)Cc1cnc(NS(=O)(=O)c2cccc(Cl)c2C)s1>>Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1
ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)OC)C.[OH-].[K+]>>ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)O)C
C[O:20][C:18]([CH2:17][c:16]1[cH:15][n:14][c:13]([NH:12][S:9]([c:8]2[c:2]([CH3:1])[c:3]([Cl:4])[cH:5][cH:6][cH:7]2)(=[O:10])=[O:11])[s:21]1)=[O:19]>>[CH3:1][c:2]1[c:3]([Cl:4])[cH:5][cH:6][cH:7][c:8]1[S:9](=[O:10])(=[O:11])[NH:12][c:13]1[n:14][cH:15][c:16]([CH2:17][C:18](=[O:19])[OH:20])[s:21]1
COC(=O)Cc1cnc(NS(=O)(=O)c2cccc(Cl)c2C)s1
Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1
null
null
CCO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=S(=O)(Nc1nccs1)c1ccccc1
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
104.9
[{"value": 97.0, "product": "ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 104.9, "product": "ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To methyl (2-{[(3-chloro-2-methylphenyl)sulfonyl]amino}-1,3-thiazol-5-yl)acetate (Example 2) (0.2 g, 0.55 mmol) dissolved in EtOH (5.5 mL) was added aqueous KOH (0.6 mL, 5.5 M). The reaction mixture was stirred at room temperature for 1 h. The solvent was then removed under reduced pressure and the crude product dissol...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1cscn1
Other
CCO
null
1
COC(=O)Cc1cnc(NS(=O)(=O)c2cccc(Cl)c2C)s1>CCO>Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d8b72c473c3d4b2989a2714c082313d6
C1COCCN1.Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1>>Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)N2CCOCC2)s1
ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)O)C.CCN=C=NCCCN(C)C.C(C)N(CC)CC.N1CCOCC1>>ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)N1CCOCC1)C
[NH:20]1[CH2:21][CH2:22][O:23][CH2:24][CH2:25]1.O[C:18]([CH2:17][c:16]1[cH:15][n:14][c:13]([NH:12][S:9]([c:8]2[c:2]([CH3:1])[c:3]([Cl:4])[cH:5][cH:6][cH:7]2)(=[O:10])=[O:11])[s:26]1)=[O:19]>>[CH3:1][c:2]1[c:3]([Cl:4])[cH:5][cH:6][cH:7][c:8]1[S:9](=[O:10])(=[O:11])[NH:12][c:13]1[n:14][cH:15][c:16]([CH2:17][C:18](=[O:19]...
C1COCCN1.Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1
Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)N2CCOCC2)s1
null
CN(C)C=1C=CN=CC1
CN(C)C=O.C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Carboxylic Acids
2ef483949e7ba3e5f888cf14cdce25fa611f75be09fdf1854a473be519821b59
c5e4172490b2731ba9322b68af56376edadc31ce0bb9a3dfdea23a1817a852fd
O=C(Cc1cnc(NS(=O)(=O)c2ccccc2)s1)N1CCOCC1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4](:[#16;a:5]):[c:6]:[#7;a:7].[#8:8]1-[C:9]-[C:10]-[NH;D2;+0:11]-[C:12]-[C:13]-1>>[#16;a:5]:[c:4](-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:11]1-[C:10]-[C:9]-[#8:8]-[C:13]-[C:12]-1):[c:6]:[#7;a:7]
10
[{"value": 10.0, "product": "ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)N1CCOCC1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 9.6, "product": "ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)N1CCOCC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of (2-{[(3-chloro-2-methylphenyl)sulfonyl]amino}-1,3-thiazol-5-yl)acetic acid (Example 3) (0.09 g, 0.25 mmol) in CH2Cl2 (5.0 mL) and DMF (0.5 mL) were added EDCI (0.05 g, 0.27 mmol), DMAP (0.02 g, 0.12 mmol), triethylamine (0.1 mL, 0.75 mmol) and morpholine (0.03 mL, 0.30 mmol). The reaction mixture was s...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Tertiary amide
C1COCCN1
C1COCC[NH]1
c1ccccc1.c1cscn1.C1COCC[NH]1
HO-
CN(C)C=1C=CN=CC1.CN(C)C=O.C(Cl)Cl
null
8
C1COCCN1.Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1>CN(C)C=1C=CN=CC1.CN(C)C=O.C(Cl)Cl>Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)N2CCOCC2)s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-38f1803929514a51a269f2c4ed9d2e97
CC(C)NC(C)C.Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1>>Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)N(C(C)C)C(C)C)s1
ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)O)C.CCN=C=NCCCN(C)C.C(C)N(CC)CC.C(C)(C)NC(C)C>>ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)N(C(C)C)C(C)C)C
[NH:20]([CH:21]([CH3:22])[CH3:23])[CH:24]([CH3:25])[CH3:26].O[C:18]([CH2:17][c:16]1[cH:15][n:14][c:13]([NH:12][S:9]([c:8]2[c:2]([CH3:1])[c:3]([Cl:4])[cH:5][cH:6][cH:7]2)(=[O:10])=[O:11])[s:27]1)=[O:19]>>[CH3:1][c:2]1[c:3]([Cl:4])[cH:5][cH:6][cH:7][c:8]1[S:9](=[O:10])(=[O:11])[NH:12][c:13]1[n:14][cH:15][c:16]([CH2:17][C...
CC(C)NC(C)C.Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1
Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)N(C(C)C)C(C)C)s1
null
CN(C)C=1C=CN=CC1
CN(C)C=O.C(Cl)Cl
Acylation
Acylation of Nitrogen Nucleophiles by Carboxylic Acids
ac72df6259d5d7baee7abdbd4706ef4b4627f86ead9dc94f0cefcfcb37c21def
c5e4172490b2731ba9322b68af56376edadc31ce0bb9a3dfdea23a1817a852fd
O=S(=O)(Nc1nccs1)c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[c:4](:[#16;a:5]):[c:6]:[#7;a:7].[C;D1;H3:8]-[C:9](-[C;D1;H3:10])-[NH;D2;+0:11]-[C:12](-[C;D1;H3:13])-[C;D1;H3:14]>>[#16;a:5]:[c:4](-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:11](-[C:9](-[C;D1;H3:8])-[C;D1;H3:10])-[C:12](-[C;D1;H3:13])-[C;D1;H3:14]):[c:6]:[#7;a:7]
9.3
[{"value": 9.0, "product": "ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)N(C(C)C)C(C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 9.3, "product": "ClC=1C(=C(C=CC1)S(=O)(=O)NC=1SC(=CN1)CC(=O)N(C(C)C)C(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of (2-{[(3-chloro-2-methylphenyl)sulfonyl]amino}-1,3-thiazol-5-yl)acetic acid (Example 3) (0.09 g, 0.25 mmol) in CH2Cl2 (5.0 mL) and DMF (0.5 mL) were added EDCI (0.05 g, 0.27 mmol), DMAP (0.02 g, 0.12 mmol), triethylamine (0.1 mL, 0.75 mmol) and diisopropylamine (0.04 mL, 0.30 mmol). The reaction mixture...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Tertiary amide
null
null
c1ccccc1.c1cscn1
HO-
CN(C)C=1C=CN=CC1.CN(C)C=O.C(Cl)Cl
null
8
CC(C)NC(C)C.Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)O)s1>CN(C)C=1C=CN=CC1.CN(C)C=O.C(Cl)Cl>Cc1c(Cl)cccc1S(=O)(=O)Nc1ncc(CC(=O)N(C(C)C)C(C)C)s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-80a2de2b1a184d3f92e129ddd5a674a8
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1>>COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
BrCC1=C(C(=O)Br)C(=CC=C1)C.[C@H]1(C[C@@H](CCC1)O)O.CC(C)([O-])C.[K+].CC1=C(C(=O)OC)C(=CC=C1)C.BrCC1=C(C(=O)OC)C(=CC=C1)C>>O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C
Br[CH2:12][c:11]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[c:6]([CH3:7])[cH:8][cH:9][cH:10]1.[OH:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([CH3:7])[cH:8][cH:9][cH:10][c:11]1[CH2:12][O:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1
COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
null
null
CN1CCCC1=O.O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
2e63de7b1f097c059f31781c5dec3b7812b761a1b3812b5238753f554cfa0846
9d3e82e8fa4f4bc62c1019e0bd869bdb0cf4748977f3c0b945b8ffdfc70126be
c1ccc(COC2CCCCC2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7].[C:8]-[C:9](-[OH;D1;+0:10])-[C:11]>>[#8:6]-[C:5](=[O;D1;H0:7])-[c:4]:[c:2](-[CH2;D2;+0:1]-[O;H0;D2;+0:10]-[C:9](-[C:8])-[C:11]):[c:3]
60
[{"value": 60.0, "product": "O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-5
CELSIUS
30
MINUTE
500 g (4.3 mol) of cis-1,3-cyclohexanediol were dissolved in 5 l of NMP and admixed with 336 g (3.0 mol) of potassium tert-butoxide (KOtBu). The internal temperature rose to 28° C. The mixture was stirred for 30 min, then cooled to −5° C. and admixed dropwise with 370 g (approx. 94%, approx. 1.4 mol) of methyl 2-bromom...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary alcohol
Ether
null
null
c1ccccc1.C1CCCCC1
HBr
CN1CCCC1=O.O
-5
0.5
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1>CN1CCCC1=O.O>COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-77fb5b5bec6a4685847a43aba0b3d881
COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1>>COC(=O)c1c(C)cccc1CO[C@@H]1CCC[C@H](O)C1
O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C>>O[C@@H]1C[C@@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C
[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([CH3:7])[cH:8][cH:9][cH:10][c:11]1[CH2:12][O:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([CH3:7])[cH:8][cH:9][cH:10][c:11]1[CH2:12][O:13][C@@H:14]1[CH2:15][CH2:16][CH2:17][C@H:18]([OH:19])[CH2:20]1
COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
COC(=O)c1c(C)cccc1CO[C@@H]1CCC[C@H](O)C1
null
null
C(C)(=O)OC=C.C(Cl)Cl
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(COC2CCCCC2)cc1
null
null
[]
null
null
28
HOUR
490 g of the crude, racemic methyl cis-2-(3-hydroxycyclohexyloxymethyl)-6-methylbenzoate (see Example 1) were dissolved in 3.1 l of methylene chloride and 850 ml of vinyl acetate, admixed with 18 g of Novozym 435 and stirred at 21–24° C. After 28 h, a further 2 g of Novozym 435 were added. After a total of 44 h, the re...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.C1CCCCC1
null
C(C)(=O)OC=C.C(Cl)Cl
null
28
COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1>C(C)(=O)OC=C.C(Cl)Cl>COC(=O)c1c(C)cccc1CO[C@@H]1CCC[C@H](O)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-dbf07741bcdc4e359660bcd6b271e077
Cc1ccc(-c2nc(COC3CCCC(O)C3)c(C)o2)cc1>>Cc1ccc(-c2nc(CO[C@@H]3CCC[C@H](O)C3)c(C)o2)cc1
CC1=CC=C(C=C1)C=1OC(=C(N1)COC1CC(CCC1)O)C>>CC1=CC=C(C=C1)C=1OC(=C(N1)CO[C@H]1C[C@H](CCC1)O)C
[CH3:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][c:8]([CH2:9][O:10][CH:11]3[CH2:12][CH2:13][CH2:14][CH:15]([OH:16])[CH2:17]3)[c:18]([CH3:19])[o:20]2)[cH:21][cH:22]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][c:8]([CH2:9][O:10][C@@H:11]3[CH2:12][CH2:13][CH2:14][C@H:15]([OH:16])[CH2:17]3)[c:18]([CH3:19])[o:20]2)[cH:21][cH:2...
Cc1ccc(-c2nc(COC3CCCC(O)C3)c(C)o2)cc1
Cc1ccc(-c2nc(CO[C@@H]3CCC[C@H](O)C3)c(C)o2)cc1
null
null
C(C)(=O)OC=C
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(-c2nc(COC3CCCCC3)co2)cc1
null
52.8
[{"value": 52.8, "product": "CC1=CC=C(C=C1)C=1OC(=C(N1)CO[C@H]1C[C@H](CCC1)O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
16.3 g of the racemic 3-[2-(4-methylphenyl)-5-methyloxazol-4-yl-methoxy]cyclohexan-1-ol were dissolved in 100 ml of vinyl acetate, admixed with 1.9 g of Chirazyme L-2, lyo., and stirred at 20–23° C. After about 30 minutes, the enzyme was filtered off and the solution concentrated under reduced pressure, crude product: ...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1cocn1.C1CCCCC1
null
C(C)(=O)OC=C
null
0.5
Cc1ccc(-c2nc(COC3CCCC(O)C3)c(C)o2)cc1>C(C)(=O)OC=C>Cc1ccc(-c2nc(CO[C@@H]3CCC[C@H](O)C3)c(C)o2)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-28284bcf97824fbea3f17da5d93ed400
Cc1oc(-c2ccccc2)nc1CO[C@@H]1CCC[C@H](O)C1>>Cc1oc(-c2ccccc2)nc1CO[C@H]1CCC[C@@H](O)C1
C1(=CC=CC=C1)C=1OC(=C(N1)CO[C@H]1C[C@H](CCC1)O)C.C[O-].[Na+].C(C)(=O)O>>C1(=CC=CC=C1)C=1OC(=C(N1)CO[C@@H]1C[C@@H](CCC1)O)C
[CH3:1][c:2]1[o:3][c:4](-[c:5]2[cH:6][cH:7][cH:8][cH:9][cH:10]2)[n:11][c:12]1[CH2:13][O:14][C@@H:15]1[CH2:16][CH2:17][CH2:18][C@H:19]([OH:20])[CH2:21]1>>[CH3:1][c:2]1[o:3][c:4](-[c:5]2[cH:6][cH:7][cH:8][cH:9][cH:10]2)[n:11][c:12]1[CH2:13][O:14][C@H:15]1[CH2:16][CH2:17][CH2:18][C@@H:19]([OH:20])[CH2:21]1
Cc1oc(-c2ccccc2)nc1CO[C@@H]1CCC[C@H](O)C1
Cc1oc(-c2ccccc2)nc1CO[C@H]1CCC[C@@H](O)C1
null
null
CO
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(-c2nc(COC3CCCCC3)co2)cc1
null
87.5
[{"value": 87.5, "product": "C1(=CC=CC=C1)C=1OC(=C(N1)CO[C@@H]1C[C@@H](CCC1)O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
0.96 g of the (1R,3S)-acetyl compound from Example 20 was dissolved in approx. 5–10 ml of MeOH, admixed with 0.1 ml of NaOMe (30%) and stirred at 20–23° C. After 3 h, the mixture was neutralized with acetic acid and concentrated under reduced pressure, taken up with ethyl acetate, washed with saturated NaHCO3, dried (M...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1cocn1.c1ccccc1.C1CCCCC1
null
CO
null
3
Cc1oc(-c2ccccc2)nc1CO[C@@H]1CCC[C@H](O)C1>CO>Cc1oc(-c2ccccc2)nc1CO[C@H]1CCC[C@@H](O)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-bdea85ef300d4da788573db5b896a3b8
CC(=O)OC1CCCC(OCc2coc(-c3ccc(F)cc3)n2)C1>>O[C@@H]1CCC[C@H](OCc2coc(-c3ccc(F)cc3)n2)C1
C(C)(=O)OC(C)=O.C(C)(=O)OC1CC(CCC1)OCC=1N=C(OC1)C1=CC=C(C=C1)F.C(CCCC(=O)[O-])(=O)OC1CC(CCC1)OCC1=CC=CC=C1.C(C1=CC=CC=C1)OC1CC(CCC1)O>>FC1=CC=C(C=C1)C=1OC=C(N1)CO[C@@H]1C[C@@H](CCC1)O
CC(=O)[O:1][CH:2]1[CH2:3][CH2:4][CH2:5][CH:6]([O:7][CH2:8][c:9]2[cH:10][o:11][c:12](-[c:13]3[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]3)[n:20]2)[CH2:21]1>>[OH:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][C@H:6]([O:7][CH2:8][c:9]2[cH:10][o:11][c:12](-[c:13]3[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]3)[n:20]2)[CH2:21]1
CC(=O)OC1CCCC(OCc2coc(-c3ccc(F)cc3)n2)C1
O[C@@H]1CCC[C@H](OCc2coc(-c3ccc(F)cc3)n2)C1
null
null
P(=O)([O-])([O-])[O-].COCCOC
Reduction
Hydrolysis or Hydrogenolysis of Carboxylic Esters or Thioesters
d7acfb2397f2b5b2a83b3bebf3698d6d984dd716982297f62a944222c79ce234
19dd58e0f83625e74b4b1375d88cb4c813ee60f593d812516d14eafc4ab68dc7
c1ccc(-c2nc(COC3CCCCC3)co2)cc1
C-C(=O)-[O;H0;D2;+0:1]-[CH;D3;+0:2](-[C:3]-[C:4])-[C:5]-[C:6]>>[C:6]-[C:5]-[C@H;D3;+0:2](-[OH;D1;+0:1])-[C:3]-[C:4]
0.1
[{"value": 0.1, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Approx. 10 mg of 3-[2-(4-fluorophenyl)oxazol-4-ylmethoxyl]cyclohexyl acetate (prepared by reacting 3-benzyloxycyclohexan-1-ol with acetic anhydride, in a similar manner to the synthesis of mono(3-benzyloxycyclohexyl) glutarate see Example 39) were taken up in 2 ml of phosphate buffer (0.1 M, pH=7.0) and 2 ml of DME and...
10.6084/m9.figshare.5104873.v1
null
Ester
Secondary alcohol
null
null
C1CCCCC1.c1cocn1.c1ccccc1
HO-
P(=O)([O-])([O-])[O-].COCCOC
null
null
CC(=O)OC1CCCC(OCc2coc(-c3ccc(F)cc3)n2)C1>P(=O)([O-])([O-])[O-].COCCOC>O[C@@H]1CCC[C@H](OCc2coc(-c3ccc(F)cc3)n2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9d65e1d4080f4e729f2a92a415415146
BrCc1ccccc1.O[C@@H]1CCC[C@H](O)C1>>O[C@H]1CCC[C@@H](OCc2ccccc2)C1
O.CC(C)([O-])C.[K+].[C@H]1(C[C@@H](CCC1)O)O.C(C1=CC=CC=C1)Br>>C(C1=CC=CC=C1)O[C@H]1C[C@H](CCC1)O
Br[CH2:8][c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1.[OH:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][C@H:6]([OH:7])[CH2:15]1>>[OH:1][C@H:2]1[CH2:3][CH2:4][CH2:5][C@@H:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1
BrCc1ccccc1.O[C@@H]1CCC[C@H](O)C1
O[C@H]1CCC[C@@H](OCc2ccccc2)C1
null
null
CN1CCCC1=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
2e63de7b1f097c059f31781c5dec3b7812b761a1b3812b5238753f554cfa0846
9d3e82e8fa4f4bc62c1019e0bd869bdb0cf4748977f3c0b945b8ffdfc70126be
c1ccc(COC2CCCCC2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6](-[OH;D1;+0:7])-[C:8]>>[C:5]-[C:6](-[O;H0;D2;+0:7]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:8]
50.6
[{"value": 50.6, "product": "C(C1=CC=CC=C1)O[C@H]1C[C@H](CCC1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
150.0 g (1.29 mol) of cis-1,3-cyclohexanediol were dissolved in 1.5 l of NMP, admixed with 111.6 g (0.99 mol) of potassium tert-butoxide (KOtBu) and stirred at 25–27° C. After about 30 minutes, the mixture was cooled to 0° C. and admixed dropwise with 78.1 g (0.46 mol) of benzyl bromide. The mixture was stirred at appr...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary alcohol
Ether
null
null
C1CCCCC1.c1ccccc1
HBr
CN1CCCC1=O
0
0.5
BrCc1ccccc1.O[C@@H]1CCC[C@H](O)C1>CN1CCCC1=O>O[C@H]1CCC[C@@H](OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b466e2935dd142b8a4e2dfd6e267d75d
O[C@H]1CCC[C@@H](OCc2ccccc2)C1>>OC1CCCC(OCc2ccccc2)C1
C(C1=CC=CC=C1)O[C@H]1C[C@H](CCC1)O>>C(C1=CC=CC=C1)OC1CC(CCC1)O
[OH:1][C@H:2]1[CH2:3][CH2:4][CH2:5][C@@H:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1>>[OH:1][CH:2]1[CH2:3][CH2:4][CH2:5][CH:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1
O[C@H]1CCC[C@@H](OCc2ccccc2)C1
OC1CCCC(OCc2ccccc2)C1
null
null
C(C)(=O)OC=C.C(Cl)Cl
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(COC2CCCCC2)cc1
null
null
[]
null
null
6
HOUR
20.3 g of cis-3-benzyloxycyclohexan-1-ol were dissolved in 35 ml of vinyl acetate and 125 ml of methylene chloride, admixed with 2.0 g of Novozym 435 and stirred at 20–23° C. for 6 h. After leaving to stand overnight, the enzyme was filtered off. A sample was withdrawn and concentrated by evaporation under reduced pres...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
C1CCCCC1.c1ccccc1
null
C(C)(=O)OC=C.C(Cl)Cl
null
6
O[C@H]1CCC[C@@H](OCc2ccccc2)C1>C(C)(=O)OC=C.C(Cl)Cl>OC1CCCC(OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3b59f332d78f46dc86667879760bad0b
O[C@H]1CCC[C@@H](OCc2ccccc2)C1>>OC1CCCC(OCc2ccccc2)C1
C(C1=CC=CC=C1)O[C@H]1C[C@H](CCC1)O>>C(C1=CC=CC=C1)OC1CC(CCC1)O
[OH:1][C@H:2]1[CH2:3][CH2:4][CH2:5][C@@H:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1>>[OH:1][CH:2]1[CH2:3][CH2:4][CH2:5][CH:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1
O[C@H]1CCC[C@@H](OCc2ccccc2)C1
OC1CCCC(OCc2ccccc2)C1
null
null
C(C)(=O)OC=C.C(Cl)Cl
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(COC2CCCCC2)cc1
null
null
[]
null
null
26
HOUR
100.0 g of cis-3-benzyloxycyclohexan-1-ol were dissolved in 170 ml of vinyl acetate and 630 ml of methylene chloride, admixed with 5.0 g of Novozym 435 and stirred at 20–23° C. for 26 h. The enzyme was filtered off, and a sample was withdrawn and concentrated by evaporation under reduced pressure. The enantiomeric exce...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
C1CCCCC1.c1ccccc1
null
C(C)(=O)OC=C.C(Cl)Cl
null
26
O[C@H]1CCC[C@@H](OCc2ccccc2)C1>C(C)(=O)OC=C.C(Cl)Cl>OC1CCCC(OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-46a2b70cb3774dc384354d92898d7d21
OC1CCCC(OCc2ccccc2)C1>>O[C@H]1CCC[C@@H](OCc2ccccc2)C1
C(C1=CC=CC=C1)OC1CC(CCC1)O>>C(C1=CC=CC=C1)O[C@H]1C[C@H](CCC1)O
[OH:1][CH:2]1[CH2:3][CH2:4][CH2:5][CH:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1>>[OH:1][C@H:2]1[CH2:3][CH2:4][CH2:5][C@@H:6]([O:7][CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1
OC1CCCC(OCc2ccccc2)C1
O[C@H]1CCC[C@@H](OCc2ccccc2)C1
null
null
CO
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(COC2CCCCC2)cc1
null
36
[{"value": 36.0, "product": "C(C1=CC=CC=C1)O[C@H]1C[C@H](CCC1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
10 g of the crude acetate/alcohol mixture from Example 29 were taken up in approx. 90 ml of methanol and approx. 70 ml of water and washed three times with in each case approx. 50 ml of n-heptane. The combined heptane phases (contain predominantly the acetate) are extracted with 50 ml of 1:1 methanol/water. The combine...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
C1CCCCC1.c1ccccc1
null
CO
null
null
OC1CCCC(OCc2ccccc2)C1>CO>O[C@H]1CCC[C@@H](OCc2ccccc2)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-39f6c4bd24b6470583618751582d3aed
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1>>COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
[C@H]1(C[C@@H](CCC1)O)O.CC(C)([O-])C.[K+].CC1=C(C(=O)OC)C(=CC=C1)C.BrCC1=C(C(=O)OC)C(=CC=C1)C>>O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C
Br[CH2:12][c:11]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[c:6]([CH3:7])[cH:8][cH:9][cH:10]1.[OH:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([CH3:7])[cH:8][cH:9][cH:10][c:11]1[CH2:12][O:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1
COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
null
null
C(C)(C)(C)OC.O.C(OC)COC
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
2e63de7b1f097c059f31781c5dec3b7812b761a1b3812b5238753f554cfa0846
9d3e82e8fa4f4bc62c1019e0bd869bdb0cf4748977f3c0b945b8ffdfc70126be
c1ccc(COC2CCCCC2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7].[C:8]-[C:9](-[OH;D1;+0:10])-[C:11]>>[#8:6]-[C:5](=[O;D1;H0:7])-[c:4]:[c:2](-[CH2;D2;+0:1]-[O;H0;D2;+0:10]-[C:9](-[C:8])-[C:11]):[c:3]
14.2
[{"value": 14.2, "product": "O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
5
CELSIUS
30
MINUTE
5 g (42.8 mmol) of cis-1,3-cyclohexanediol were dissolved in 50 ml of dimethoxyethane (DME), admixed at 20–23° C. with 3.36 g (30 mmol) of potassium tert-butoxide (KOtBu) and stirred. After about 30 minutes, the mixture is cooled to 5° C. and 3.7 g (approx. 50%) of methyl 2-bromomethyl-6-methylbenzoate, which may be pr...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary alcohol
Ether
null
null
c1ccccc1.C1CCCCC1
HBr
C(C)(C)(C)OC.O.C(OC)COC
5
0.5
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1>C(C)(C)(C)OC.O.C(OC)COC>COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-34aac6db739c484d8d628fa15ea117fa
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1>>COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
[C@H]1(C[C@@H](CCC1)O)O.CC1=C(C(=O)OC)C(=CC=C1)C.BrCC1=C(C(=O)OC)C(=CC=C1)C.BrCC1=C(C(=O)Br)C(=CC=C1)C.CC(C)([O-])C.[K+]>>O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C
Br[CH2:12][c:11]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[c:6]([CH3:7])[cH:8][cH:9][cH:10]1.[OH:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([CH3:7])[cH:8][cH:9][cH:10][c:11]1[CH2:12][O:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1
COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
null
null
C(C)(C)(C)OC.O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
2e63de7b1f097c059f31781c5dec3b7812b761a1b3812b5238753f554cfa0846
9d3e82e8fa4f4bc62c1019e0bd869bdb0cf4748977f3c0b945b8ffdfc70126be
c1ccc(COC2CCCCC2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7].[C:8]-[C:9](-[OH;D1;+0:10])-[C:11]>>[#8:6]-[C:5](=[O;D1;H0:7])-[c:4]:[c:2](-[CH2;D2;+0:1]-[O;H0;D2;+0:10]-[C:9](-[C:8])-[C:11]):[c:3]
14.2
[{"value": 14.2, "product": "O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
5
CELSIUS
30
MINUTE
10.0 g (86 mmol) of cis-1,3-cyclohexanediol were taken up in 150 ml of methyl tert-butyl ether (MTBE), admixed at approx. 20° C. with 6.72 g (59.9 mmol) of potassium tert-butoxide (KOtBu) and stirred. After about 30 minutes, the suspension was cooled to 5° C. and admixed dropwise with 7.4 g (approx. 50%) of methyl 2-br...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary alcohol
Ether
null
null
c1ccccc1.C1CCCCC1
HBr
C(C)(C)(C)OC.O
5
0.5
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1>C(C)(C)(C)OC.O>COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-65ef42f140954425a031aa8adb08d3a5
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1>>COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
O.CC(C)([O-])C.[K+].[C@H]1(C[C@@H](CCC1)O)O.BrCC1=C(C(=O)OC)C(=CC=C1)C>>O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C
Br[CH2:12][c:11]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[c:6]([CH3:7])[cH:8][cH:9][cH:10]1.[OH:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([CH3:7])[cH:8][cH:9][cH:10][c:11]1[CH2:12][O:13][C@H:14]1[CH2:15][CH2:16][CH2:17][C@@H:18]([OH:19])[CH2:20]1
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1
COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
null
null
CN1C(N(CCC1)C)=O.ClC1=CC=CC=C1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
2e63de7b1f097c059f31781c5dec3b7812b761a1b3812b5238753f554cfa0846
9d3e82e8fa4f4bc62c1019e0bd869bdb0cf4748977f3c0b945b8ffdfc70126be
c1ccc(COC2CCCCC2)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](-[#8:6])=[O;D1;H0:7].[C:8]-[C:9](-[OH;D1;+0:10])-[C:11]>>[#8:6]-[C:5](=[O;D1;H0:7])-[c:4]:[c:2](-[CH2;D2;+0:1]-[O;H0;D2;+0:10]-[C:9](-[C:8])-[C:11]):[c:3]
13.7
[{"value": 13.7, "product": "O[C@H]1C[C@H](CCC1)OCC1=C(C(=O)OC)C(=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
5 g (42.8 mmol) of cis-1,3-cyclohexanediol were dissolved in 40 ml of chlorobenzene and 10 ml of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (DMPU, dimethylpropyleneurea), admixed at 20–23° C. with 3.36 g (30 mmol) of potassium tert-butoxide (KOtBu) and stirred. After 10–15 minutes, the mixture was cooled to 15–...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary alcohol
Ether
null
null
c1ccccc1.C1CCCCC1
HBr
CN1C(N(CCC1)C)=O.ClC1=CC=CC=C1
null
null
COC(=O)c1c(C)cccc1CBr.O[C@@H]1CCC[C@H](O)C1>CN1C(N(CCC1)C)=O.ClC1=CC=CC=C1>COC(=O)c1c(C)cccc1CO[C@H]1CCC[C@@H](O)C1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-47a6823fceb64ef4b003a8a5ae160266
Cc1ccc(C=O)cc1.O.O>>Cc1ccc(C(O)C(=O)O)cc1
C(Cl)(Cl)Cl.C1(=CC=C(C=C1)C=O)C.[OH-].[Na+].O.[OH-].[Na+].O>>CC1=CC=C(C(C(=O)O)O)C=C1
[CH3:1][c:2]1[cH:3][cH:4][c:5]([CH:6]=[O:7])[cH:11][cH:12]1.[OH2:9].[OH2:10]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([CH:6]([OH:7])[C:8](=[O:9])[OH:10])[cH:11][cH:12]1
Cc1ccc(C=O)cc1.O.O
Cc1ccc(C(O)C(=O)O)cc1
null
[Cl-].C(C1=CC=CC=C1)[N+](CC)(CC)CC
null
Acylation
OtherReaction
e4754e3793ba0362af7cd262e2f320471fced6da69cfa59aaf69349f987b0106
7b79ddb9582ae558ef0424125dcd16c236a764b78e4d8d3057436676b03c02cd
c1ccccc1
[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5].[OH2;D0;+0:6].[OH2;D0;+0:7]>>[O;H0;D1;+0:6]=[C:8](-[OH;D1;+0:7])-[CH;D3;+0:2](-[OH;D1;+0:1])-[c:3](:[c:4]):[c:5]
null
[]
10
CELSIUS
6
HOUR
A 300 gal reactor was charged with water (150 L) and sodium hydroxide (100 kg) and the solution was cooled to 10±5° C. A second 300 gal reactor was charged with chloroform (203 kg), benzyltriethylammonium chloride (8.2 kg) and 4-tolualdehyde (99 kg). The reaction mixture was heated to gentle reflux and the sodium hydro...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Carboxylic acid.Secondary alcohol
null
null
c1ccccc1
Other
[Cl-].C(C1=CC=CC=C1)[N+](CC)(CC)CC
10
6
Cc1ccc(C=O)cc1.O.O>[Cl-].C(C1=CC=CC=C1)[N+](CC)(CC)CC>Cc1ccc(C(O)C(=O)O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1a5375979fb5402d8fe980b291f4b317
Cc1ccc(C2(C(=O)O)CC2C(=O)O)cc1.NC(N)=O>>Cc1ccc(C23CC2C(=O)NC3=O)cc1
CC1=CC=C(C=C1)C1(C(C1)C(=O)O)C(=O)O.NC(=O)N>>CC1=CC=C(C=C1)C12C(NC(C2C1)=O)=O
O[C:9]([CH:8]1[C:6]([c:5]2[cH:4][cH:3][c:2]([CH3:1])[cH:15][cH:14]2)([C:12](O)=[O:13])[CH2:7]1)=[O:10].NC(=O)[NH2:11]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([C:6]23[CH2:7][CH:8]2[C:9](=[O:10])[NH:11][C:12]3=[O:13])[cH:14][cH:15]1
Cc1ccc(C2(C(=O)O)CC2C(=O)O)cc1.NC(N)=O
Cc1ccc(C23CC2C(=O)NC3=O)cc1
null
null
C1(=CC=CC=C1)C
Acylation
OtherReaction
f102f31968cec5a5cce8a63f187e2c2787ad6463f06ec6d023228eecad5281ab
5eb28b4134086b781d00fd84897bce5d880f3b8a3f2763256df6a2d491a6f5b2
O=C1NC(=O)C2(c3ccccc3)CC12
N-C(=O)-[NH2;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4]1(-[c:5])-[C:6]-[C:7]-1-[C;H0;D3;+0:8](-O)=[O;D1;H0:9]>>[O;D1;H0:9]=[C;H0;D3;+0:8]1-[NH;D2;+0:1]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4]2(-[c:5])-[C:6]-[C:7]-1-2
null
[]
null
null
null
null
A mixture of purified 1-(4-methylphenyl)-1,2-cyclopropanedicarboxylic acid (58 kg), toluene (465 kg) and urea (23.8 kg) was heated to reflux and the mixture held at reflux until the reaction was complete. On completion of the reaction period, the solution was cooled to 80–90° C. and washed with water (69 L). The lower ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Carboxylic acid.Urea
Unsubstituted dicarboximide
null
C1NCC2CC12
c1ccccc1.C1NCC2CC12
HO-
C1(=CC=CC=C1)C
null
null
Cc1ccc(C2(C(=O)O)CC2C(=O)O)cc1.NC(N)=O>C1(=CC=CC=C1)C>Cc1ccc(C23CC2C(=O)NC3=O)cc1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c509486ce7d542aeba24813fa375ce8e
CCOC(=O)CC(=O)Cl.Nc1ccc(Br)cc1S.O=S1C=Nc2ccc(Br)cc21.O=S1C=Nc2ccc(Br)cc21.[OH-]>>CCOC(=O)C1=C(O)Nc2ccc(Br)cc2S1.CCOC(=O)Cc1nc2ccc(Br)cc2s1
NC1=C(C=C(C=C1)Br)S.C(C)OC(CC(=O)Cl)=O.BrC1=CC2=C(N=CS2=O)C=C1.BrC1=CC2=C(N=CS2=O)C=C1.[OH-].[Na+]>>C(C)OC(CC=1SC2=C(N1)C=CC(=C2)Br)=O.C(C)OC(=O)C=1SC2=C(NC1O)C=CC(=C2)Br
Cl[C:21](=[O:22])[CH2:23][C:4]([O:3][CH2:2][CH3:1])=[O:5].[NH2:25][c:26]1[cH:27][cH:28][c:29]([Br:30])[cH:31][c:32]1[SH:33].[CH:7]1=[N:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]2[S:17]1=[O:8].O=S1[c:6]2cc(Br)[cH:18][cH:19]c2N=[CH:24]1.[OH-:20]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]1=[C:7]([OH:8])[NH:9][c:10]2[...
CCOC(=O)CC(=O)Cl.Nc1ccc(Br)cc1S.O=S1C=Nc2ccc(Br)cc21.O=S1C=Nc2ccc(Br)cc21.[OH-]
CCOC(=O)C1=C(O)Nc2ccc(Br)cc2S1.CCOC(=O)Cc1nc2ccc(Br)cc2s1
null
null
null
C-C Coupling
OtherReaction
bf0ea44699cc37e70c3e03e5bc2ee44e1fc39c23a4fbe8e0f3af1c0cf28c15a5
c986c860b0f4e047419b8e2b347702ba5635b8e1e85b19f8c1ec6852237aadeb
C1=CSc2ccccc2N1.c1ccc2scnc2c1
Br-c1:[cH;D2;+0:1]:[cH;D2;+0:2]:c2:[c;H0;D3;+0:3](:c:1)-S(=O)-[CH;D2;+0:4]=N-2.Cl-[C;H0;D3;+0:5](=[O;D1;H0:6])-[CH2;D2;+0:7]-[C;H0;D3;+0:8](=[O;D1;H0:9])-[#8:10]-[C:11].[NH2;D1;+0:12]-[c:13](:[c:14]):[c:15](-[SH;D1;+0:16]):[c:17].[O;H0;D1;+0:18]=[S;H0;D3;+0:19]1-[CH;D2;+0:20]=[N;H0;D2;+0:21]-[c:22](:[c:23]):[c:24]-1:[c...
null
[]
null
null
null
null
Compounds of formula (22) can be prepared from 6-bromobenzothiazolone as shown in Scheme 3. 6-Bromobenzothiazolone is heated in the presence of NaOH base to provide a mixture of 2-amino-5-bromothiophenol (15) and its disulfide (16). The mixture is treated with chlorocarbonyl-acetic acid ethyl ester to provide 6-bromo-b...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Aromatic halide.Ester.Primary amine.Aromatic thiol.Sulfoxide.Sulfoxide
Enamine.Ester.Ester.Enol.Monosulfide
c1ccccc1.c1ccc2scnc2c1.c1ccc2scnc2c1
C1=CSc2ccccc2N1.c1ccc2scnc2c1
C1=CSc2ccccc2N1.c1ccc2scnc2c1
HCl.Br-
null
null
null
CCOC(=O)CC(=O)Cl.Nc1ccc(Br)cc1S.O=S1C=Nc2ccc(Br)cc21.O=S1C=Nc2ccc(Br)cc21.[OH-]>>CCOC(=O)C1=C(O)Nc2ccc(Br)cc2S1.CCOC(=O)Cc1nc2ccc(Br)cc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-22bb215d286d4b7dacf3111b06283fce
CCOC(=O)Cc1nc2ccc(Br)cc2s1>>OCCc1nc2ccc(Br)cc2s1
C(C)OC(CC=1SC2=C(N1)C=CC(=C2)Br)=O.[BH4-].[Na+]>>BrC1=CC2=C(N=C(S2)CCO)C=C1
CCO[C:2](=[O:1])[CH2:3][c:4]1[n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][c:12]2[s:13]1>>[OH:1][CH2:2][CH2:3][c:4]1[n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][c:12]2[s:13]1
CCOC(=O)Cc1nc2ccc(Br)cc2s1
OCCc1nc2ccc(Br)cc2s1
null
null
null
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc2scnc2c1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]-[c:4](:[#16;a:5]):[#7;a:6]>>[#16;a:5]:[c:4](-[C:3]-[CH2;D2;+0:1]-[OH;D1;+0:2]):[#7;a:6]
null
[]
null
null
null
null
Compounds of formula (22) can be prepared from 6-bromobenzothiazolone as shown in Scheme 3. 6-Bromobenzothiazolone is heated in the presence of NaOH base to provide a mixture of 2-amino-5-bromothiophenol (15) and its disulfide (16). The mixture is treated with chlorocarbonyl-acetic acid ethyl ester to provide 6-bromo-b...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccc2scnc2c1
HO-
null
null
null
CCOC(=O)Cc1nc2ccc(Br)cc2s1>>OCCc1nc2ccc(Br)cc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-8fbb89cd170e414183553eb3fcd55f41
CS(=O)(=O)Cl.OCCc1nc2ccc(Br)cc2s1>>CS(=O)(=O)OCCc1nc2ccc(Br)cc2s1
BrC1=CC2=C(N=C(S2)CCO)C=C1.S(=O)(=O)(C)Cl>>BrC1=CC2=C(N=C(S2)CCOS(=O)(=O)C)C=C1
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][CH2:7][c:8]1[n:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]2[s:17]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][CH2:7][c:8]1[n:9][c:10]2[cH:11][cH:12][c:13]([Br:14])[cH:15][c:16]2[s:17]1
CS(=O)(=O)Cl.OCCc1nc2ccc(Br)cc2s1
CS(=O)(=O)OCCc1nc2ccc(Br)cc2s1
null
null
C(C)N(CC)CC
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1ccc2scnc2c1
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: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]
null
[]
null
null
null
null
Compounds of formula (22) can be prepared from 6-bromobenzothiazolone as shown in Scheme 3. 6-Bromobenzothiazolone is heated in the presence of NaOH base to provide a mixture of 2-amino-5-bromothiophenol (15) and its disulfide (16). The mixture is treated with chlorocarbonyl-acetic acid ethyl ester to provide 6-bromo-b...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1ccc2scnc2c1
HCl
C(C)N(CC)CC
null
null
CS(=O)(=O)Cl.OCCc1nc2ccc(Br)cc2s1>C(C)N(CC)CC>CS(=O)(=O)OCCc1nc2ccc(Br)cc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4a3b06cd55a14560b4976cfed5f06416
C#CCCN1CCCC1C.Nc1ccc(Br)cc1I>>CC1CCCN1CCC#Cc1cc(Br)ccc1N
C(CC#C)N1C(CCC1)C.BrC1=CC(=C(C=C1)N)I>>BrC1=CC(=C(C=C1)N)C#CCCN1C(CCC1)C
[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][C:9]#[CH:10].I[c:11]1[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]1[NH2:18]>>[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][C:9]#[C:10][c:11]1[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]1[NH2:18]
C#CCCN1CCCC1C.Nc1ccc(Br)cc1I
CC1CCCN1CCC#Cc1cc(Br)ccc1N
null
null
null
C-C Coupling
Sonogashira alkyne_aryl halide
15c08902746c61a960c314898ce6bb5fcc5e189f9e057388c59dba9ec9d0c81c
305eca0fd2975da49e7f69e4edfb9dc1cbce82513954bc5a73be3289e70e5f76
C(#Cc1ccccc1)CCN1CCCC1
I-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[N;D1;H2:5]):[c:6].[C:7]-[C:8]#[CH;D1;+0:9]>>[C:7]-[C:8]#[C;H0;D2;+0:9]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[N;D1;H2:5]):[c:6]
null
[]
null
null
null
null
The compound of formula (43) can be prepared from 3-butynyl p-toluenesulfonate (42) and 2(R)-methylpyrrrolidine L-tartrate (40) as shown in Scheme 5. 2(R)-Methylpyrrolidine L-tartrate (40) is treated with potassium carbonate in acetonitrile to provide 2(R)-methylpyrrolidine (41), which is combined with 3-butynyl p-tolu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Alkyne
Alkyne
c1ccccc1
c1ccccc1
C1CC[NH]C1.c1ccccc1
HI
null
null
null
C#CCCN1CCCC1C.Nc1ccc(Br)cc1I>>CC1CCCN1CCC#Cc1cc(Br)ccc1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d7024dd9e5254cfbaa00ffa5e9ae3740
CC1CCCN1CCc1nc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1>>CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
BrC1=CC2=C(NC(=N2)CCN2C(CCC2)C)C=C1.BrC1=CC2=C(NC(=N2)CCN2C(CCC2)C)C=C1.C(#N)C1=CC=C(C=C1)B(O)O>>CC1N(CCC1)CCC1=NC2=C(N1)C=CC(=C2)C2=CC=C(C#N)C=C2
Br[c:13]1[cH:12][c:11]2[n:10][c:9]([CH2:8][CH2:7][N:6]3[CH:2]([CH3:1])[CH2:3][CH2:4][CH2:5]3)[nH:25][c:24]2[cH:23][cH:22]1.OB(O)[c:14]1[cH:15][cH:16][c:17]([C:18]#[N:19])[cH:20][cH:21]1>>[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13](-[c:14]3[cH:15][cH:16][c:17]([C:18]#[N:19])[c...
CC1CCCN1CCc1nc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1
CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
null
null
null
C-C Coupling
Suzuki coupling with boronic acids
4c01b75ced48e0c5dbfbda4cb6a596e9d3a1d181f4aef3fbd9604232ef2322c4
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3[nH]c(CCN4CCCC4)nc3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:2:[c:8]:[c:9]:1.O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]>>[c:12]:[c:11]:[c;H0;D3;+0:10](-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:2:[c:8]:[c:9]:1):[c:13]:[c:14]
null
[]
null
null
null
null
Compounds of formula (55) and (55a) can be prepared from 2(R)-methylpyrrolidine HCl (50) and ethyl acrylate (51) as shown in Scheme 6. 2(R)-Methylpyrrolidine HCl can be treated with potassium carbonate to provide 2(R)-methylpyrrolidine (41), which is reacted with ethyl acrylate (51) to provide 3-(2-methyl-pyrrolidin-1-...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2[nH]cnc2c1.c1ccccc1
c1ccc2[nH]cnc2c1.c1ccccc1
C1CC[NH]C1.c1ccc2[nH]cnc2c1.c1ccccc1
HBr.B
null
null
null
CC1CCCN1CCc1nc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1>>CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e468895d0537455791117c5aa46e01fd
CC(C)(C)OC(=O)N1CC[C@H]1CO.CS(=O)(=O)Cl>>CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O
C([O-])(O)=O.[Na+].C(C)(C)(C)OC(=O)N1[C@@H](CC1)CO.C(C)N(CC)CC.CS(=O)(=O)Cl>>C(C)(C)(C)OC(=O)N1[C@@H](CC1)COS(=O)(=O)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C@H:11]1[CH2:12][OH:13].Cl[S:14]([CH3:15])(=[O:16])=[O:17]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C@H:11]1[CH2:12][O:13][S:14]([CH3:15])(=[O:16])=[O:17]
CC(C)(C)OC(=O)N1CC[C@H]1CO.CS(=O)(=O)Cl
CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O
null
null
ClCCl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
C1CNC1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#7:5]-[C:6]-[C:7]-[OH;D1;+0:8]>>[#7:5]-[C:6]-[C:7]-[O;H0;D2;+0:8]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4]
null
[]
0
CELSIUS
8
HOUR
2-(S)-Hydroxymethyl-azetidine-1-carboxylic acid tert-butyl ester (prepared as described in Abreo, et al. J. Med. Chem. 1996, 39, 817–825) (9.7 g, 52 mmol) was taken up in dichloromethane (50 mL), treated with triethylamine (8.7 mL, 62 mmol), cooled to 0° C., treated dropwise with methanesulfonyl chloride (4.4 mL, 57 mm...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
C1C[NH]C1
HCl
ClCCl
0
8
CC(C)(C)OC(=O)N1CC[C@H]1CO.CS(=O)(=O)Cl>ClCCl>CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-98a2701b80cf40f4b520ee3818c90065
CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O>>C[C@@H]1CCN1C(=O)OC(C)(C)C
C(C)(C)(C)OC(=O)N1[C@@H](CC1)COS(=O)(=O)C.C(C)[BH-](CC)CC.[Li+].C(C)(=O)OCC>>C(C)(C)(C)OC(=O)N1[C@@H](CC1)C
CS(=O)(=O)O[CH2:1][C@@H:2]1[CH2:3][CH2:4][N:5]1[C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12]>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][N:5]1[C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12]
CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O
C[C@@H]1CCN1C(=O)OC(C)(C)C
null
null
C1CCOC1
Functional Group Interconversion
OtherReaction
b912c78cb197e36ec1377256b010930a62c194e425d624f79bd79646c51988b4
28e81ae8a7ce8bef7c0a5c5aadad67636bd3c9bf494add5caa6f4f660788ae85
C1CNC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]1-[C:3]-[C:4]-[#7:5]-1-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12]>>[C;D1;H3:10]-[C:9](-[C;D1;H3:11])(-[C;D1;H3:12])-[#8:8]-[C:6](=[O;D1;H0:7])-[#7:5]1-[C:4]-[C:3]-[C:2]-1-[CH3;D1;+0:1]
30
[{"value": 30.0, "product": "C(C)(C)(C)OC(=O)N1[C@@H](CC1)C", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
6
HOUR
2-(S)-Methanesulfonyloxymethyl-azetidine-1-carboxylic acid tert-butyl ester was (4.83 g, 18.2 mmol) was taken up in THF (11 mL), cooled to 0° C. under N2, treated drop-wise with a lithium triethylborohydride (1.0 M in THF, 73 mL), stirred at ambient temperature for 6 hours, treated with ethyl acetate (500 mL), washed w...
10.6084/m9.figshare.5104873.v1
null
Mesylate
null
null
null
C1C[NH]C1
MsOH.HO-
C1CCOC1
0
6
CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O>C1CCOC1>C[C@@H]1CCN1C(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d77490cfe1ed472b8c43e116c87aa2d2
CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O.[F-]>>CC(C)(C)OC(=O)N1CC[C@H]1CF
C(C)(C)(C)OC(=O)N1[C@@H](CC1)COS(=O)(=O)C.[F-].C(CCC)[N+](CCCC)(CCCC)CCCC>>C(C)(C)(C)OC(=O)N1[C@@H](CC1)CF
CS(=O)(=O)O[CH2:12][C@H:11]1[N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][CH2:10]1.[F-:13]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C@H:11]1[CH2:12][F:13]
CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O.[F-]
CC(C)(C)OC(=O)N1CC[C@H]1CF
null
null
null
Functional Group Interconversion
OtherReaction
119410ad0456baafba3b2935b12d3e44977c506a6dd8cacdd3e4fe37abe9db9f
ddf832dd4937bef392b42ed4281006ae20524cc7fc61b350edeb12d7b5bf783f
C1CNC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]1-[C:3]-[C:4]-[#7:5]-1-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12].[F-;H0;D0:13]>>[C;D1;H3:10]-[C:9](-[C;D1;H3:11])(-[C;D1;H3:12])-[#8:8]-[C:6](=[O;D1;H0:7])-[#7:5]1-[C:4]-[C:3]-[C:2]-1-[CH2;D2;+0:1]-[F;H0;D1;+0:13]
null
[]
null
null
null
null
2-(S)-Methanesulfonyloxymethyl-azetidine-1-carboxylic acid tert-butyl ester (5.62 g, 21.2 mmol) was treated with tetrabutylammonium fluoride (1 M solution in THF, 191 mL) under N2, heated to reflux for 1 hour, cooled to ambient temperature, concentrated to 50 mL, treated with water (100 mL) and extracted with ethyl ace...
10.6084/m9.figshare.5104873.v1
null
Mesylate
Primary halide
null
null
C1C[NH]C1
MsOH.HO-
null
null
null
CC(C)(C)OC(=O)N1CC[C@H]1COS(C)(=O)=O.[F-]>>CC(C)(C)OC(=O)N1CC[C@H]1CF
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1090695690f74685a1dece36db0314be
C=O.Cc1nc2cc(Br)ccc2s1>>OCCc1nc2cc(Br)ccc2s1
BrC=1C=CC2=C(N=C(S2)C)C1.[NH4+].[Cl-].[Li]N1C(CCCC1(C)C)(C)C.[Li]CCCC.C=O>>BrC=1C=CC2=C(N=C(S2)CCO)C1
[O:1]=[CH2:2].[CH3:3][c:4]1[n:5][c:6]2[cH:7][c:8]([Br:9])[cH:10][cH:11][c:12]2[s:13]1>>[OH:1][CH2:2][CH2:3][c:4]1[n:5][c:6]2[cH:7][c:8]([Br:9])[cH:10][cH:11][c:12]2[s:13]1
C=O.Cc1nc2cc(Br)ccc2s1
OCCc1nc2cc(Br)ccc2s1
null
null
C1CCOC1
C-C Coupling
OtherReaction
e09a7c53ddc9875d8ca974c0a8ce2e05d5a94c87ff882117809becd87c4c217b
4396295d899f5d4f5de2e844a80fc7d194b4da158f49df3d2717206b401b59bd
c1ccc2scnc2c1
[CH2;D1;+0:1]=[O;H0;D1;+0:2].[CH3;D1;+0:3]-[c:4]1:[#16;a:5]:[c:6]:[c:7]:[#7;a:8]:1>>[OH;D1;+0:2]-[CH2;D2;+0:1]-[CH2;D2;+0:3]-[c:4]1:[#16;a:5]:[c:6]:[c:7]:[#7;a:8]:1
null
[]
-78
CELSIUS
3
HOUR
To a dry 100 mL flask, 2,2,6′,6′-tetra-methyl piperidine (0.56 g, 4 mmol) and 6 mL of THF was added and cooled to −78° C. Then n-BuLi (1.5 mL, 2.5M) was added rapidly, and the mixture of LiTMP was stirred for 3 hr. 5-Bromo-2-methyl-benzothiazole (0.75 g, 3.3 mmol) was added in solid form in to the reaction at −78° C., ...
10.6084/m9.figshare.5104873.v1
null
Formaldehyde
Primary alcohol
null
null
c1ccc2scnc2c1
null
C1CCOC1
-78
3
C=O.Cc1nc2cc(Br)ccc2s1>C1CCOC1>OCCc1nc2cc(Br)ccc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ab2cc805775c4093bee9592abaf35306
CS(=O)(=O)Cl.OCCc1nc2cc(Br)ccc2s1>>CS(=O)(=O)OCCc1nc2cc(Br)ccc2s1
CS(=O)(=O)Cl.BrC=1C=CC2=C(N=C(S2)CCO)C1.CCN(CC)CC>>BrC=1C=CC2=C(N=C(S2)CCOS(=O)(=O)C)C1
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][CH2:7][c:8]1[n:9][c:10]2[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]2[s:17]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][CH2:7][c:8]1[n:9][c:10]2[cH:11][c:12]([Br:13])[cH:14][cH:15][c:16]2[s:17]1
CS(=O)(=O)Cl.OCCc1nc2cc(Br)ccc2s1
CS(=O)(=O)OCCc1nc2cc(Br)ccc2s1
null
null
C(Cl)Cl
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
c1ccc2scnc2c1
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: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]
null
[]
null
null
null
null
To a mixture of 2-(5-bromo-benzothiazol-2-yl)-ethanol (0.94 g, 3.6 mmol) in 10 mL CH2Cl2, Et3N (0.99 g, 9.8 mmol), was added methanesulfonyl chloride (0.46 g, 4.0 mmol) dropwise at room temperature. The reaction was worked up by concentrating under vacuum and then used in the next step, Example 1C. Conditions: See reac...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
c1ccc2scnc2c1
HCl
C(Cl)Cl
null
null
CS(=O)(=O)Cl.OCCc1nc2cc(Br)ccc2s1>C(Cl)Cl>CS(=O)(=O)OCCc1nc2cc(Br)ccc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3a282d85555e47b2bfce6f9522c00967
CS(=O)(=O)OCCc1nc2cc(Br)ccc2s1.C[C@@H]1CCCN1>>C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2s1
CCN(CC)CC.BrC=1C=CC2=C(N=C(S2)CCOS(=O)(=O)C)C1.C[C@H]1NCCC1>>BrC=1C=CC2=C(N=C(S2)CCN2[C@@H](CCC2)C)C1
CS(=O)(=O)O[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[s:18]1.[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][NH:6]1>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[s:18]1
CS(=O)(=O)OCCc1nc2cc(Br)ccc2s1.C[C@@H]1CCCN1
C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2s1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
Alkylation of amines
d27d68bc3d43f6d66a205fa71d9985c3ff34906c317c31aac4632a55b7f79861
35d789812c3241c3a185d06663a309d930259e30563212f3884ef74718436cbc
c1ccc2sc(CCN3CCCC3)nc2c1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[c:3](:[#16;a:4]):[#7;a:5].[C;D1;H3:6]-[C:7]1-[C:8]-[C:9]-[C:10]-[NH;D2;+0:11]-1>>[#16;a:4]:[c:3](-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:11]1-[C:10]-[C:9]-[C:8]-[C:7]-1-[C;D1;H3:6]):[#7;a:5]
null
[]
60
CELSIUS
null
null
The methanesulfonic acid 2-(5-bromo-benzothiazol)-2-yl)-ethyl ester from Example 1B, and 2 equivalents (7.3 mmol) of 2-(R)-methyl pyrrolidine (at a concentration of 10 mg/mL solution in acetonitrile), was combined with excess Et3N (0.99 g, 9.8 mmol), and the resulting mixture was heated to 60° C. for 2 hr. The solvent ...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Secondary amine
Tertiary amine
C1CCNC1
C1CC[NH]C1
C1CC[NH]C1.c1ccc2scnc2c1
MsOH.HO-
C(C)#N
60
null
CS(=O)(=O)OCCc1nc2cc(Br)ccc2s1.C[C@@H]1CCCN1>C(C)#N>C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-edb4a5288d3a40f7b9ddd0afc3612493
CC1CCCN1CCc1nc2cc(Br)ccc2s1.N#Cc1ccc(B(O)O)cc1>>CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2s1
C(=O)([O-])[O-].[K+].[K+].[F-].[Cs+].C(#N)C1=CC=C(C=C1)B(O)O.C1(CCCCC1)P(C1=C(C=CC=C1)C1=CC=CC=C1)C1CCCCC1.BrC=1C=CC2=C(N=C(S2)CCN2C(CCC2)C)C1>>CC1N(CCC1)CCC=1SC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2
Br[c:13]1[cH:12][c:11]2[n:10][c:9]([CH2:8][CH2:7][N:6]3[CH:2]([CH3:1])[CH2:3][CH2:4][CH2:5]3)[s:25][c:24]2[cH:23][cH:22]1.OB(O)[c:14]1[cH:15][cH:16][c:17]([C:18]#[N:19])[cH:20][cH:21]1>>[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13](-[c:14]3[cH:15][cH:16][c:17]([C:18]#[N:19])[cH...
CC1CCCN1CCc1nc2cc(Br)ccc2s1.N#Cc1ccc(B(O)O)cc1
CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2s1
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]
C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
dafc139bc4494937b580450e1f22e20f12d86e297a18c2a2ce8a2d9de753d94b
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3sc(CCN4CCCC4)nc3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[#16;a:6]:[c:7]:2:[c:8]:[c:9]:1.O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]>>[c:12]:[c:11]:[c;H0;D3;+0:10](-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[#16;a:6]:[c:7]:2:[c:8]:[c:9]:1):[c:13]:[c:14]
31.5
[{"value": 31.5, "product": "CC1N(CCC1)CCC=1SC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2", "details": "PERCENTYIELD", "is_desired": false}]
90
CELSIUS
null
null
To a reaction flask containing K2CO3 (0.326 g, 1.5 mmol), CsF (0.233 g, 1.5 mmol), and (0.19 g, 1.3 mmol) of 4-cyanophenyl boronic acid was added a solution of 5-bromo-2-[2-(2-methyl-pyrrolidin-1-yl)-ethyl]-benzothiazole (0.25 g, 0.77 mmol) in 3 mL of toluene. The resulting mixture was purged with nitrogen, and then 2-...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2scnc2c1.c1ccccc1
c1ccc2scnc2c1.c1ccccc1
C1CC[NH]C1.c1ccc2scnc2c1.c1ccccc1
HBr.B
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C1(=CC=CC=C1)C
90
null
CC1CCCN1CCc1nc2cc(Br)ccc2s1.N#Cc1ccc(B(O)O)cc1>C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].C1(=CC=CC=C1)C>CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-047fe1c5f9834cbcb16b3e4e1a1cbfb3
O=[N+]([O-])c1cc(Br)ccc1S>>Nc1cc(Br)ccc1S
BrC1=CC(=C(C=C1)S)[N+](=O)[O-].BrC1=CC(=C(C=C1)S)[N+](=O)[O-].[H][H]>>NC1=C(C=CC(=C1)Br)S
O=[N+:1]([O-])[c:2]1[cH:3][c:4]([Br:5])[cH:6][cH:7][c:8]1[SH:9]>>[NH2:1][c:2]1[cH:3][c:4]([Br:5])[cH:6][cH:7][c:8]1[SH:9]
O=[N+]([O-])c1cc(Br)ccc1S
Nc1cc(Br)ccc1S
null
[Ni]
C1CCOC1
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccccc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
The mixture of 4-bromo-2-nitro-benzenethiol and its disulfide from Example 2A (14.9 g, 53.5 mmol) in THF (450 mL) was mixed with Raney Ni (30 g, 100% wt). The mixture was hydrogenated in a 1000 mL Paar shaker at a hydrogen pressure of 40 psi at 50° C. for 41 hours. When the reaction was complete, the solids were filter...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1
Other
[Ni].C1CCOC1
null
null
O=[N+]([O-])c1cc(Br)ccc1S>[Ni].C1CCOC1>Nc1cc(Br)ccc1S
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-98cc223bf38a4ce9a090aa143a53649e
CCOC(=O)Cc1nc2cc(Br)ccc2s1>>OCCc1nc2cc(Br)ccc2s1
C(C)OC(CC=1SC2=C(N1)C=C(C=C2)Br)=O.[BH4-].[Na+]>>BrC=1C=CC2=C(N=C(S2)CCO)C1
CCO[C:2](=[O:1])[CH2:3][c:4]1[n:5][c:6]2[cH:7][c:8]([Br:9])[cH:10][cH:11][c:12]2[s:13]1>>[OH:1][CH2:2][CH2:3][c:4]1[n:5][c:6]2[cH:7][c:8]([Br:9])[cH:10][cH:11][c:12]2[s:13]1
CCOC(=O)Cc1nc2cc(Br)ccc2s1
OCCc1nc2cc(Br)ccc2s1
null
null
C1CCOC1.CCO
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc2scnc2c1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]-[c:4](:[#16;a:5]):[#7;a:6]>>[#16;a:5]:[c:4](-[C:3]-[CH2;D2;+0:1]-[OH;D1;+0:2]):[#7;a:6]
null
[]
null
null
2
HOUR
(5-Bromo-benzothiazol-2-yl)-acetic acid ethyl ester (1.25 g, 4.2 mmol) was dissolved in THF (20 mL) and EtOH (5 mL) under N2. Then 0.24 g of NaBH4 was dissolved in EtOH (3 mL) and added to the above solution. The reaction mixture was stirred at room temperature for 2 hours. After the completion the mixture was quenched...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccc2scnc2c1
HO-
C1CCOC1.CCO
null
2
CCOC(=O)Cc1nc2cc(Br)ccc2s1>C1CCOC1.CCO>OCCc1nc2cc(Br)ccc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-648115ee2be148f0b50d9bf80b823d53
CC#N.CCN(CC)CC.CS(=O)(=O)Cl.OCCc1nc2cc(Br)ccc2s1>>C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2s1
BrC=1C=CC2=C(N=C(S2)CCO)C1.C(C)N(CC)CC.C(C)#N.C(C)N(CC)CC.S(=O)(=O)(C)Cl>>BrC=1C=CC2=C(N=C(S2)CCN2[C@@H](CCC2)C)C1
[C:2]([CH3:3])#[N:6].CCN(CC)[CH2:5][CH3:4].O=S(=O)(Cl)[CH3:1].O[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[s:18]1>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[s:18]1
CC#N.CCN(CC)CC.CS(=O)(=O)Cl.OCCc1nc2cc(Br)ccc2s1
C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2s1
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
OtherReaction
e5920dee39fd4e23ef47b22853f6a079fe3f61b5f6e67d8ed9ea1517aa09b86a
161a415a813f397cd540024355cb50c7cef50673b6c8766c860bc7e640c38f0d
c1ccc2sc(CCN3CCCC3)nc2c1
C-C-N(-C-C)-[CH2;D2;+0:1]-[CH3;D1;+0:2].Cl-S(=O)(=O)-[CH3;D1;+0:3].O-[CH2;D2;+0:4]-[C:5]-[c:6](:[#16;a:7]):[#7;a:8].[CH3;D1;+0:9]-[C;H0;D2;+0:10]#[N;H0;D1;+0:11]>>[#16;a:7]:[c:6](-[C:5]-[CH2;D2;+0:4]-[N;H0;D3;+0:11]1-[CH2;D2;+0:1]-[CH2;D2;+0:2]-[CH2;D2;+0:9]-[C@H;D3;+0:10]-1-[CH3;D1;+0:3]):[#7;a:8]
100
[{"value": 100.0, "product": "BrC=1C=CC2=C(N=C(S2)CCN2[C@@H](CCC2)C)C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A solution of 2-(5-bromo-benzothiazol-2-yl)-ethanol (1.50 g, 5.8 mmol) and triethylamine (1.33 g, 11.6 mmol) in CH2Cl2 was cooled to 0° C., and mesyl chloride was added dropwise. The mixture was warmed to room temperature and stirred for 1 hr. The solvent was removed under vacuum, and to the residue was added acetonitr...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Primary alcohol.Tertiary amine.Sulfonyl halide
Tertiary amine
null
C1CC[NH]C1
C1CC[NH]C1.c1ccc2scnc2c1
HCl
C(Cl)Cl
null
1
CC#N.CCN(CC)CC.CS(=O)(=O)Cl.OCCc1nc2cc(Br)ccc2s1>C(Cl)Cl>C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9e0a998deb1f41e6be0b5926a4440d62
CCOC(=O)C1=C(O)Nc2ccc(Br)cc2S1>>CCOC(=O)Cc1nc2ccc(Br)cc2s1
C(C)OC(=O)C=1SC2=C(NC1O)C=CC(=C2)Br>>C(C)OC(CC=1SC2=C(N1)C=CC(=C2)Br)=O
O[C:7]1=[C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[S:16][c:15]2[c:9]([cH:10][cH:11][c:12]([Br:13])[cH:14]2)[NH:8]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][c:7]1[n:8][c:9]2[cH:10][cH:11][c:12]([Br:13])[cH:14][c:15]2[s:16]1
CCOC(=O)C1=C(O)Nc2ccc(Br)cc2S1
CCOC(=O)Cc1nc2ccc(Br)cc2s1
null
[Zn]
C(C)(=O)O
Miscellaneous
OtherReaction
fc649200af8e1ad1b1d9f8e7005a8ae3b629126f30b62ef8211b8ab6436e3821
84800cecbc2734529d618fbe9e9bfc0f092a255228f2e6c590042cef943220a2
c1ccc2scnc2c1
O-[C;H0;D3;+0:1]1=[C;H0;D3;+0:2](-[C:3](=[O;D1;H0:4])-[#8:5]-[C:6])-[S;H0;D2;+0:7]-[c:8](:[c:9]):[c:10](:[c:11])-[NH;D2;+0:12]-1>>[C:6]-[#8:5]-[C:3](=[O;D1;H0:4])-[CH2;D2;+0:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:12]:[c:10](:[c:11]):[c:8](:[c:9]):[s;H0;D2;+0:7]:1
null
[]
110
CELSIUS
2
HOUR
7-Bromo-3-hydroxy-4H-benzo[1,4]thiazine-2-carboxylic acid ethyl ester (2.47 g, 7.8 mmol) was dissolved in 50 mL of acetic acid and heated to 110° C. under nitrogen. Zinc powder (7.5 g, 114.7 mmol) was added in portions at room temperature over 80 minutes. The mixture was stirred at 110° C. for additional 2 hours and co...
10.6084/m9.figshare.5104873.v1
null
Enamine.Ester.Enol.Monosulfide
Ester
C1=CSc2ccccc2N1
c1ccc2scnc2c1
c1ccc2scnc2c1
Other
[Zn].C(C)(=O)O
110
2
CCOC(=O)C1=C(O)Nc2ccc(Br)cc2S1>[Zn].C(C)(=O)O>CCOC(=O)Cc1nc2ccc(Br)cc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d81361375ed643d0b99a999c148fc8ac
CCOC(=O)Cc1nc2ccc(Br)cc2s1>>OCCc1nc2ccc(Br)cc2s1
[BH4-].[Na+].C(C)OC(CC=1SC2=C(N1)C=CC(=C2)Br)=O>>BrC1=CC2=C(N=C(S2)CCO)C=C1
CCO[C:2](=[O:1])[CH2:3][c:4]1[n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][c:12]2[s:13]1>>[OH:1][CH2:2][CH2:3][c:4]1[n:5][c:6]2[cH:7][cH:8][c:9]([Br:10])[cH:11][c:12]2[s:13]1
CCOC(=O)Cc1nc2ccc(Br)cc2s1
OCCc1nc2ccc(Br)cc2s1
null
null
C1CCOC1.C(C)O
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc2scnc2c1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]-[c:4](:[#16;a:5]):[#7;a:6]>>[#16;a:5]:[c:4](-[C:3]-[CH2;D2;+0:1]-[OH;D1;+0:2]):[#7;a:6]
null
[]
null
null
15
HOUR
To a stirred mixture of sodium borohydride (1.11 g, 29.3 mmol) in ethanol (10 mL) at room temperature was added a solution of the (6-bromo-benzothiazol-2-yl)-acetic acid ethyl ester (2.2 g, 7.3 mmol) in THF (25 mL) at 23–28° C. The mixture was stirred at room temperature for 15 hr, cooled to 3° C. and quenched with 20 ...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccc2scnc2c1
HO-
C1CCOC1.C(C)O
null
15
CCOC(=O)Cc1nc2ccc(Br)cc2s1>C1CCOC1.C(C)O>OCCc1nc2ccc(Br)cc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-9edf0410addf43d4bed914c8f716366e
C[C@@H]1CCCN1.OCCc1nc2ccc(Br)cc2s1>>CC1CCCN1CCc1nc2ccc(Br)cc2s1
BrC1=CC2=C(N=C(S2)CCO)C=C1.C(C)N(CC)CC.C([O-])([O-])=O.[K+].[K+].Cl.C[C@H]1NCCC1.S(=O)(=O)(C)Cl>>BrC1=CC2=C(N=C(S2)CCN2C(CCC2)C)C=C1
[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][NH:6]1.O[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]2[s:18]1>>[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]2[s:18]1
C[C@@H]1CCCN1.OCCc1nc2ccc(Br)cc2s1
CC1CCCN1CCc1nc2ccc(Br)cc2s1
null
null
C1CCOC1.C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
5b5461e2c999b5ff4ebd02389aabcfa6da1d5461f5b1011870f0b8680e19702d
87693a475e46c41583976158ec46dcaf8be8cc05c5635654a6a68033770f8d5c
c1ccc2sc(CCN3CCCC3)nc2c1
O-[CH2;D2;+0:1]-[C:2]-[c:3](:[#16;a:4]):[#7;a:5].[C;D1;H3:6]-[C@@H;D3;+0:7]1-[C:8]-[C:9]-[C:10]-[NH;D2;+0:11]-1>>[#16;a:4]:[c:3](-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:11]1-[C:10]-[C:9]-[C:8]-[CH;D3;+0:7]-1-[C;D1;H3:6]):[#7;a:5]
88.7
[{"value": 88.3, "product": "BrC1=CC2=C(N=C(S2)CCN2C(CCC2)C)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 88.7, "product": "BrC1=CC2=C(N=C(S2)CCN2C(CCC2)C)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A solution of 2-(6-bromo-benzothiazol-2-yl)-ethanol (2.23 g, 8.6 mmol) and triethylamine (2.19 g, 21.6 mmol) in THF (45 mL) was cooled to −20° C., and mesyl chloride (1.58 g, 13.8 mmol) was added at −20 to −10° C. The mixture was warmed to room temperature and stirred for 2 hr. Potassium carbonate (1.79 g, 13 mmol), 2-...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Secondary amine
Tertiary amine
C1CCNC1
C1CC[NH]C1
C1CC[NH]C1.c1ccc2scnc2c1
HO-
C1CCOC1.C(C)#N
null
2
C[C@@H]1CCCN1.OCCc1nc2ccc(Br)cc2s1>C1CCOC1.C(C)#N>CC1CCCN1CCc1nc2ccc(Br)cc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e7d8686f93f04837b803ce8e0f3a19eb
C[C@@H]1CCCN1CCc1nc2ccc(Br)cc2s1.OB(O)c1cccnc1>>C[C@@H]1CCCN1CCc1nc2ccc(-c3cccnc3)cc2s1
BrC1=CC2=C(N=C(S2)CCN2[C@@H](CCC2)C)C=C1.N1=CC(=CC=C1)B(O)O.C1(CCCCC1)P(C1=C(C=CC=C1)C1=CC=CC=C1)C1CCCCC1.C([O-])([O-])=O.[Na+].[Na+]>>C[C@H]1N(CCC1)CCC=1SC2=C(N1)C=CC(=C2)C=2C=NC=CC2
Br[c:14]1[cH:13][cH:12][c:11]2[n:10][c:9]([CH2:8][CH2:7][N:6]3[C@H:2]([CH3:1])[CH2:3][CH2:4][CH2:5]3)[s:23][c:22]2[cH:21]1.OB(O)[c:15]1[cH:16][cH:17][cH:18][n:19][cH:20]1>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][cH:13][c:14](-[c:15]3[cH:16][cH:17][cH:18][n:19][cH:20]3)[cH:21]...
C[C@@H]1CCCN1CCc1nc2ccc(Br)cc2s1.OB(O)c1cccnc1
C[C@@H]1CCCN1CCc1nc2ccc(-c3cccnc3)cc2s1
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
O.CC(C)O
C-C Coupling
Suzuki coupling with boronic acids
c70fee0da30dc36b8a4bebab6ea83795444d7fd4b4a174e37bfe6a9f9425b533
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1cncc(-c2ccc3nc(CCN4CCCC4)sc3c2)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]2:[#7;a:5]:[c:6]:[#16;a:7]:[c:8]:2:[c:9]:1.O-B(-O)-[c;H0;D3;+0:10]1:[c:11]:[c:12]:[c:13]:[#7;a:14]:[c:15]:1>>[#16;a:7]1:[c:6]:[#7;a:5]:[c:4]2:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:10]3:[c:11]:[c:12]:[c:13]:[#7;a:14]:[c:15]:3):[c:9]:[c:8]:1:2
68.7
[{"value": 67.0, "product": "C[C@H]1N(CCC1)CCC=1SC2=C(N1)C=CC(=C2)C=2C=NC=CC2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 68.7, "product": "C[C@H]1N(CCC1)CCC=1SC2=C(N1)C=CC(=C2)C=2C=NC=CC2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
65
CELSIUS
null
null
A mixture of 6-bromo-2-[2-(2-(R)-methyl-pyrrolidin-1-yl)-ethyl]-benzothiazole (0.3 g, 0.9 mmol), 3-pyridinyl boronic acid (0.17 g, 1.4 mmol) and 2-(dicyclohexylphosphino)biphenyl (65 mg, 0.2 mmol) in 15 mL of IPA was purged wth nitrogen. Dichlorobis(triphenylphosphine)palladium II (65 mg, 0.1 mmol) was added. Sodium ca...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2scnc2c1.c1ccncc1
c1ccc2scnc2c1.c1ccncc1
C1CC[NH]C1.c1ccc2scnc2c1.c1ccncc1
HBr.B
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.O.CC(C)O
65
null
C[C@@H]1CCCN1CCc1nc2ccc(Br)cc2s1.OB(O)c1cccnc1>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.O.CC(C)O>C[C@@H]1CCCN1CCc1nc2ccc(-c3cccnc3)cc2s1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-1c01067372e44b6680ad32e1a7caf277
C=CC(=O)O.Nc1cc(Br)ccc1O>>C=Cc1nc2cc(Br)ccc2o1
C(C=C)(=O)O.NC1=C(C=CC(=C1)Br)O.CS(=O)(=O)O.O=P12OP3(=O)OP(=O)(O1)OP(=O)(O2)O3.[OH-].[Na+]>>BrC=1C=CC2=C(N=C(O2)C=C)C1
O=[C:3](O)[CH:2]=[CH2:1].[NH2:4][c:5]1[cH:6][c:7]([Br:8])[cH:9][cH:10][c:11]1[OH:12]>>[CH2:1]=[CH:2][c:3]1[n:4][c:5]2[cH:6][c:7]([Br:8])[cH:9][cH:10][c:11]2[o:12]1
C=CC(=O)O.Nc1cc(Br)ccc1O
C=Cc1nc2cc(Br)ccc2o1
null
null
ClCCl.O.C(C)OCC
Aromatic Heterocycle Formation
Benzoxazole formation from ester/carboxylic acid
ab90945f453b9d98729e6912eac27527ccc8f6879f9fc67f913646675914d5f8
082415a064525fb5ab1054c8f1a07a8509dc65297c7337b4b21c60d0aec70378
c1ccc2ocnc2c1
O-[C;H0;D3;+0:1](=O)-[C:2]=[C;D1;H2:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[c:7](-[OH;D1;+0:8]):[c:9]>>[C;D1;H2:3]=[C:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:4]:[c:5](:[c:6]):[c:7](:[c:9]):[o;H0;D2;+0:8]:1
45.1
[{"value": 45.0, "product": "BrC=1C=CC2=C(N=C(O2)C=C)C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 45.1, "product": "BrC=1C=CC2=C(N=C(O2)C=C)C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
78
CELSIUS
12
HOUR
A mixture of 12 g of methanesulfonic acid and 1.8 g of phosphorus pentoxide (P2O5) was stirred 12 hours. To this well stirred suspension was added 0.346 g (4.8 mmol) of acrylic acid and 0.808 g (4 mmol) of 2-amino-4-bromo-phenol. The reaction was heated at 78° C. for 5 hours, then cooled to room temperature. The reacti...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Aromatic alcohol.Primary amine
null
c1ccccc1
c1ccc2ocnc2c1
c1ccc2ocnc2c1
HO-
ClCCl.O.C(C)OCC
78
12
C=CC(=O)O.Nc1cc(Br)ccc1O>ClCCl.O.C(C)OCC>C=Cc1nc2cc(Br)ccc2o1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-28e2094b51fe4314ac393822d96728b9
C=Cc1nc2cc(Br)ccc2o1.N#Cc1ccc(B(O)O)cc1>>C=Cc1nc2cc(-c3ccc(C#N)cc3)ccc2o1
BrC=1C=CC2=C(N=C(O2)C=C)C1.C(#N)C1=CC=C(C=C1)B(O)O.C(C)(C)(C)P(C(C)(C)C)C(C)(C)C.O1CCCC1>>C(=C)C=1OC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2
Br[c:7]1[cH:6][c:5]2[n:4][c:3]([CH:2]=[CH2:1])[o:19][c:18]2[cH:17][cH:16]1.OB(O)[c:8]1[cH:9][cH:10][c:11]([C:12]#[N:13])[cH:14][cH:15]1>>[CH2:1]=[CH:2][c:3]1[n:4][c:5]2[cH:6][c:7](-[c:8]3[cH:9][cH:10][c:11]([C:12]#[N:13])[cH:14][cH:15]3)[cH:16][cH:17][c:18]2[o:19]1
C=Cc1nc2cc(Br)ccc2o1.N#Cc1ccc(B(O)O)cc1
C=Cc1nc2cc(-c3ccc(C#N)cc3)ccc2o1
null
null
CCCCCC
C-C Coupling
Suzuki coupling with boronic acids
99bf694f84e9ec22cb82f9819557cd37221283254ff798499273a8b4f21eaca4
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3ocnc3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]2:[#8;a:5]:[c:6](-[C:7]=[C;D1;H2:8]):[#7;a:9]:[c:10]:2:[c:11]:1.O-B(-O)-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]>>[C;D1;H2:8]=[C:7]-[c:6]1:[#7;a:9]:[c:10]2:[c:11]:[c;H0;D3;+0:1](-[c;H0;D3;+0:12](:[c:13]:[c:14]):[c:15]:[c:16]):[c:2]:[c:3]:[c:4]:2:[#8;a:5]:1
78
[{"value": 78.0, "product": "C(=C)C=1OC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.0, "product": "C(=C)C=1OC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
23
CELSIUS
24
HOUR
A mixture of 224 mg (1 mmol) of 5-bromo-2-vinyl-benzooxazole, 191 mg (1.3 mmol) of 4-cyanophenylboronic acid, 55 mg (0.03 mmol) of tris-(dibenzylidineacetone)dipalladium (0) (CAS #52409-22-0), 0.2 mL (0.06 mmol) of a 10% solution of tri-tert-butylphosphine in hexane, and 1.5 mL of tetrahydrofuran was stirred at 23° C. ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2ocnc2c1.c1ccccc1
c1ccc2ocnc2c1.c1ccccc1
c1ccc2ocnc2c1.c1ccccc1
HBr.B
CCCCCC
23
24
C=Cc1nc2cc(Br)ccc2o1.N#Cc1ccc(B(O)O)cc1>CCCCCC>C=Cc1nc2cc(-c3ccc(C#N)cc3)ccc2o1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-066231d855314bf3955d22c323fbe57e
C=Cc1nc2cc(-c3ccc(C#N)cc3)ccc2o1.CC1CCCN1>>CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2o1
C(=C)C=1OC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2.CC1NCCC1>>CC1N(CCC1)CCC=1OC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2
[CH2:7]=[CH:8][c:9]1[n:10][c:11]2[cH:12][c:13](-[c:14]3[cH:15][cH:16][c:17]([C:18]#[N:19])[cH:20][cH:21]3)[cH:22][cH:23][c:24]2[o:25]1.[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][NH:6]1>>[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13](-[c:14]3[cH:15][cH:16][c:17]([C:18]#[N:19])[cH:20][cH...
C=Cc1nc2cc(-c3ccc(C#N)cc3)ccc2o1.CC1CCCN1
CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2o1
null
null
C(C)O
Heteroatom Alkylation and Arylation
aza-Michael addition secondary
dd05e02f89f4334a0cbf67e5033d2677d654bbf2f6f7ab2436d63d82eac8e490
828fcbb87adfef9f22c9a1e52b43c3df76cb2e49bfe62b57e8b79965772a2bed
c1ccc(-c2ccc3oc(CCN4CCCC4)nc3c2)cc1
[C;D1;H3:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[NH;D2;+0:6]-1.[CH2;D1;+0:7]=[CH;D2;+0:8]-[c:9]1:[#7;a:10]:[c:11]:[c:12]:[#8;a:13]:1>>[C;D1;H3:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[N;H0;D3;+0:6]-1-[CH2;D2;+0:7]-[CH2;D2;+0:8]-[c:9]1:[#7;a:10]:[c:11]:[c:12]:[#8;a:13]:1
100
[{"value": 100.0, "product": "CC1N(CCC1)CCC=1OC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.6, "product": "CC1N(CCC1)CCC=1OC2=C(N1)C=C(C=C2)C2=CC=C(C#N)C=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 24.6 mg (0.1 mmol) of 4-(2-vinyl-benzooxazol-5-yl)-benzonitrile and 24 mg of racemic 2-methyl-pyrrolidine (Aldrich, CAS #765-38-8) in 0.25 mL of ethanol was stirred at room temperature for 1 hour, then concentrated in vacuo to a glass to give pure product racemic 4-{2-[2-(2-methyl-pyrrolidin-1-yl)-ethyl]-...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Vinyl
Tertiary amine
C1CCNC1
C1CC[NH]C1
C1CC[NH]C1.c1ccc2ocnc2c1.c1ccccc1
null
C(C)O
null
null
C=Cc1nc2cc(-c3ccc(C#N)cc3)ccc2o1.CC1CCCN1>C(C)O>CC1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2o1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-aaf4f21a45734751b2c179840ecdc207
C#CCCOS(=O)(=O)c1ccc(C)cc1.C[C@@H]1CCCN1>>C#CCCN1CCC[C@H]1C
C(=O)(O)[C@H](O)[C@@H](O)C(=O)O.C[C@H]1NCCC1.C1(=CC=C(C=C1)S(=O)(=O)OCCC#C)C.C([O-])([O-])=O.[K+].[K+]>>C(CC#C)N1[C@@H](CCC1)C
Cc1ccc(S(=O)(=O)O[CH2:4][CH2:3][C:2]#[CH:1])cc1.[NH:5]1[CH2:6][CH2:7][CH2:8][C@H:9]1[CH3:10]>>[CH:1]#[C:2][CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][CH2:8][C@H:9]1[CH3:10]
C#CCCOS(=O)(=O)c1ccc(C)cc1.C[C@@H]1CCCN1
C#CCCN1CCC[C@H]1C
null
null
CC#N
Heteroatom Alkylation and Arylation
OtherReaction
bdf21feb16e238d3a4e1a225eabe2c616c4f3ccb3286bcf173af5a52d353d303
71b4ac4449ece5e0df64e56caf0f1cbac76e83f802a92104cfb6c6c861b6a71c
C1CCNC1
C-c1:c:c:c(-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[C:3]#[C;D1;H1:4]):c:c:1.[C;D1;H3:5]-[C:6]1-[C:7]-[C:8]-[C:9]-[NH;D2;+0:10]-1>>[C;D1;H1:4]#[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:10]1-[C:9]-[C:8]-[C:7]-[C:6]-1-[C;D1;H3:5]
null
[]
85
CELSIUS
null
null
To a sealed flask was added 2-(R)-methylpyrrolidine L-tartrate (21.1 g, 90 mmol), 3-butynyl p-toluenesulfonate (15.7 mL, 89 mmol), potassium carbonate powder (18.5 g, 134 mmol) and CH3CN (160 mL). The resulting mixture was heated to 85° C. for 24 hours and the reaction was monitored by GC for the complete consumption o...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Secondary amine
Tertiary amine
c1ccccc1.C1CCNC1
C1CC[NH]C1
C1CC[NH]C1
TsOH.HO-
CC#N
85
null
C#CCCOS(=O)(=O)c1ccc(C)cc1.C[C@@H]1CCCN1>CC#N>C#CCCN1CCC[C@H]1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-3e0d8478526940bf83b3ecdefee834a4
C#CCCN1CCC[C@H]1C.Nc1ccc(Br)cc1I>>C[C@@H]1CCCN1CCC#Cc1cc(Br)ccc1N
C#CC(C)N1C(CCC1)C.C(CC#C)N1[C@@H](CCC1)C.BrC1=CC(=C(C=C1)N)I.C(C)(C)NC(C)C.BrC1=CC(=C(C=C1)N)I>>BrC1=CC(=C(C=C1)N)C#CCCN1[C@@H](CCC1)C
[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][C:9]#[CH:10].I[c:11]1[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]1[NH2:18]>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][C:9]#[C:10][c:11]1[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]1[NH2:18]
C#CCCN1CCC[C@H]1C.Nc1ccc(Br)cc1I
C[C@@H]1CCCN1CCC#Cc1cc(Br)ccc1N
null
[Cu]I.BrC=1C=CC2=C(N=C(S2)CCO)C1
null
C-C Coupling
Sonogashira alkyne_aryl halide
15c08902746c61a960c314898ce6bb5fcc5e189f9e057388c59dba9ec9d0c81c
305eca0fd2975da49e7f69e4edfb9dc1cbce82513954bc5a73be3289e70e5f76
C(#Cc1ccccc1)CCN1CCCC1
I-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[N;D1;H2:5]):[c:6].[C:7]-[C:8]#[CH;D1;+0:9]>>[C:7]-[C:8]#[C;H0;D2;+0:9]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[N;D1;H2:5]):[c:6]
97.3
[{"value": 97.3, "product": "BrC1=CC(=C(C=C1)N)C#CCCN1[C@@H](CCC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a solution of 1-butyn-3-yl-2-methyl-pyrrolidine in CH3CN (prepared in Example 65A assuming 100% conversion, 89 mmol) was added 4-bromo-2-iodo-phenylamine (12.0 g, 40 mmol) under nitrogen followed by addition of CuI (0.38 g, 2.0 mmol), PdCl2(PPh3) 2 (0.70 mg, 1.0 mmol) and diisopropylamine (33.6 mL, 240 mmol). The re...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Alkyne
Alkyne
c1ccccc1
c1ccccc1
C1CC[NH]C1.c1ccccc1
HI
[Cu]I.BrC=1C=CC2=C(N=C(S2)CCO)C1
null
2
C#CCCN1CCC[C@H]1C.Nc1ccc(Br)cc1I>[Cu]I.BrC=1C=CC2=C(N=C(S2)CCO)C1>C[C@@H]1CCCN1CCC#Cc1cc(Br)ccc1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-20fcc1c0ad4341a8a27727e3d8993f13
CC1CCCN1CCC#Cc1cc(Br)ccc1N>>C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2[nH]1
O([K])C(C)(C)C.BrC1=CC(=C(C=C1)N)C#CCCN1C(CCC1)C>>BrC=1C=C2C=C(NC2=CC1)CCN1[C@@H](CCC1)C
[CH3:1][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][C:9]#[C:10][c:11]1[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]1[NH2:18]>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[cH:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[nH:18]1
CC1CCCN1CCC#Cc1cc(Br)ccc1N
C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2[nH]1
null
null
CN1CCCC1=O
Aromatic Heterocycle Formation
OtherReaction
3eeece0a35b6fca4def8d3bd74336b0b713b6a44d29870eaf5592e4f702c94e8
f32b9a5ecc70d866a53cd56f9bc47b365771cdcbb02563cae8c78e4de228d870
c1ccc2[nH]c(CCN3CCCC3)cc2c1
[C:1]-[C:2]-[C;H0;D2;+0:3]#[C;H0;D2;+0:4]-[c:5](:[c:6]):[c:7](-[NH2;D1;+0:8]):[c:9]>>[C:1]-[C:2]-[c;H0;D3;+0:3]1:[cH;D2;+0:4]:[c:5](:[c:6]):[c:7](:[c:9]):[nH;D2;+0:8]:1
61.2
[{"value": 61.2, "product": "BrC=1C=C2C=C(NC2=CC1)CCN1[C@@H](CCC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a cooled (0° C.) suspension of KO-tBu (95%, 7.8 g, 66 mmol) in NMP (150 mL) was added a solution of 4-bromo-2-[4-(2-methyl-pyrrolidin-1-yl)-but-1-ynyl]-phenylamine (10 g, 33 mmol) in NMP (50 mL) dropwise keeping the temperature below 5° C. The resulting mixture was then stirred at room temperature for 3 hours under ...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Alkyne
null
c1ccccc1
c1ccc2[nH]ccc2c1
C1CC[NH]C1.c1ccc2[nH]ccc2c1
null
CN1CCCC1=O
null
3
CC1CCCN1CCC#Cc1cc(Br)ccc1N>CN1CCCC1=O>C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2[nH]1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-f6fabe9f122d4790935ad38391ad854e
C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1>>C[C@@H]1CCCN1CCc1cc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
BrC=1C=C2C=C(NC2=CC1)CCN1[C@@H](CCC1)C.C(=O)([O-])[O-].[Cs+].[Cs+].[F-].[Cs+].C(#N)C1=CC=C(C=C1)B(O)O.C1(CCCCC1)P(C1=C(C=CC=C1)C1=CC=CC=C1)C1CCCCC1>>C[C@H]1N(CCC1)CCC=1NC2=CC=C(C=C2C1)C1=CC=C(C#N)C=C1
Br[c:13]1[cH:12][c:11]2[cH:10][c:9]([CH2:8][CH2:7][N:6]3[C@H:2]([CH3:1])[CH2:3][CH2:4][CH2:5]3)[nH:25][c:24]2[cH:23][cH:22]1.OB(O)[c:14]1[cH:15][cH:16][c:17]([C:18]#[N:19])[cH:20][cH:21]1>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[cH:10][c:11]2[cH:12][c:13](-[c:14]3[cH:15][cH:16][c:17]([C:18]#[N:1...
C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1
C[C@@H]1CCCN1CCc1cc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
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]
O.C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
42e21206f0250bb469664981cf521bd21ce6ff7bf8a8e9271f94397f7d3b79cb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3[nH]c(CCN4CCCC4)cc3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6]:[c:7]:1.O-B(-O)-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]):[c:7]:[c:6]:1
44.9
[{"value": 44.9, "product": "C[C@H]1N(CCC1)CCC=1NC2=CC=C(C=C2C1)C1=CC=C(C#N)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
65
CELSIUS
null
null
A reaction flask was charged with Cs2CO3 (1.14 g, 3.5 mmol), CsF (0.38 g, 2.5 mmol), 4-cyanophenylboronic acid (425 mg, 2.5 mmol), and H2O (10 mL) followed by a toluene solution (10 mL) of 5-bromo-2-[2-(2-(R)-methyl-pyrrolidin-1-yl)-ethyl]-1H-indole (307 mg, 1.0 mmol). The resulting mixture was purged with nitrogen. To...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2[nH]ccc2c1.c1ccccc1
c1ccc2[nH]ccc2c1.c1ccccc1
C1CC[NH]C1.c1ccc2[nH]ccc2c1.c1ccccc1
HBr.B
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].O.C1(=CC=CC=C1)C
65
null
C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1>C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].O.C1(=CC=CC=C1)C>C[C@@H]1CCCN1CCc1cc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-248bde4b2f92454f832a0d25b1c7fe81
CI.C[C@@H]1CCCN1CCC#Cc1cc(Br)ccc1N>>C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2n1C
N1C=CC2=CC=CC=C12.O([K])C(C)(C)C.BrC1=CC(=C(C=C1)N)C#CCCN1[C@@H](CCC1)C.CI>>BrC=1C=C2C=C(N(C2=CC1)C)CCN1[C@@H](CCC1)C
I[CH3:19].[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][C:9]#[C:10][c:11]1[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]1[NH2:18]>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[cH:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[n:18]1[CH3:19]
CI.C[C@@H]1CCCN1CCC#Cc1cc(Br)ccc1N
C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2n1C
null
null
CN1CCCC1=O.O
Aromatic Heterocycle Formation
OtherReaction
3eeece0a35b6fca4def8d3bd74336b0b713b6a44d29870eaf5592e4f702c94e8
f32b9a5ecc70d866a53cd56f9bc47b365771cdcbb02563cae8c78e4de228d870
c1ccc2[nH]c(CCN3CCCC3)cc2c1
I-[CH3;D1;+0:1].[C:2]-[C:3]-[C;H0;D2;+0:4]#[C;H0;D2;+0:5]-[c:6](:[c:7]):[c:8](-[NH2;D1;+0:9]):[c:10]>>[C:2]-[C:3]-[c;H0;D3;+0:4]1:[cH;D2;+0:5]:[c:6](:[c:7]):[c:8](:[c:10]):[n;H0;D3;+0:9]:1-[CH3;D1;+0:1]
89.8
[{"value": 89.8, "product": "BrC=1C=C2C=C(N(C2=CC1)C)CCN1[C@@H](CCC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a cooled (0° C.) suspension of KO-tBu (95%, 6.2 g, 52 mmol) in NMP (120 mL) was added a solution of 4-bromo-2-[4-(2-(R)-methyl-pyrrolidin-1-yl)-but-1-ynyl]-phenylamine (8.0 g, 26 mmol) in NMP (50 mL) dropwise keeping the temperature below 5° C. The resulting mixture was then stirred at roan temperature for 3 hours u...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Alkyne
null
c1ccccc1
c1ccc2[nH]ccc2c1
C1CC[NH]C1.c1ccc2[nH]ccc2c1
HI
CN1CCCC1=O.O
null
3
CI.C[C@@H]1CCCN1CCC#Cc1cc(Br)ccc1N>CN1CCCC1=O.O>C[C@@H]1CCCN1CCc1cc2cc(Br)ccc2n1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e374225418be4187b8abb583b3fe848e
CC1CCCN1CCc1cc2cc(Br)ccc2n1C.N#Cc1ccc(B(O)O)cc1>>C[C@@H]1CCCN1CCc1cc2cc(-c3ccc(C#N)cc3)ccc2n1C
BrC=1C=C2C=C(N(C2=CC1)C)CCN1C(CCC1)C.BrC=1C=C2C=C(N(C2=CC1)C)CCN1C(CCC1)C.C(=O)([O-])[O-].[Cs+].[Cs+].[F-].[Cs+].C(#N)C1=CC=C(C=C1)B(O)O>>CN1C(=CC2=CC(=CC=C12)C1=CC=C(C#N)C=C1)CCN1[C@@H](CCC1)C
Br[c:13]1[cH:12][c:11]2[cH:10][c:9]([CH2:8][CH2:7][N:6]3[CH:2]([CH3:1])[CH2:3][CH2:4][CH2:5]3)[n:25]([CH3:26])[c:24]2[cH:23][cH:22]1.OB(O)[c:14]1[cH:15][cH:16][c:17]([C:18]#[N:19])[cH:20][cH:21]1>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[cH:10][c:11]2[cH:12][c:13](-[c:14]3[cH:15][cH:16][c:17]([C:...
CC1CCCN1CCc1cc2cc(Br)ccc2n1C.N#Cc1ccc(B(O)O)cc1
C[C@@H]1CCCN1CCc1cc2cc(-c3ccc(C#N)cc3)ccc2n1C
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]
O.C1(=CC=CC=C1)C
C-C Coupling
Suzuki coupling with boronic acids
42e21206f0250bb469664981cf521bd21ce6ff7bf8a8e9271f94397f7d3b79cb
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3[nH]c(CCN4CCCC4)cc3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](:[#7;a:5]):[c:6]:[c:7]:1.O-B(-O)-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]>>[#7;a:5]:[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12]):[c:7]:[c:6]:1
44.8
[{"value": 44.8, "product": "CN1C(=CC2=CC(=CC=C12)C1=CC=C(C#N)C=C1)CCN1[C@@H](CCC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
65
CELSIUS
null
null
A reaction flask was charged with Cs2CO3 (1.14 g, 3.5 mmol), CsF (0.38 g, 2.5 mmol), 4-cyanophenylboronic acid (425 mg, 2.5 mmol), and H2O (10 mL) followed by a toluene solution (10 mL) of 5-bromo-1-methyl-2-[2-(2-methyl-pyrrolidin-1-yl)-ethyl]-1H-indole (320 mg, 1.0 mmol). The resulting mixture was purged with nitroge...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2[nH]ccc2c1.c1ccccc1
c1ccc2[nH]ccc2c1.c1ccccc1
C1CC[NH]C1.c1ccc2[nH]ccc2c1.c1ccccc1
HBr.B
C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].O.C1(=CC=CC=C1)C
65
null
CC1CCCN1CCc1cc2cc(Br)ccc2n1C.N#Cc1ccc(B(O)O)cc1>C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.C=1C=CC(=CC1)/C=C/C(=O)/C=C/C2=CC=CC=C2.[Pd].[Pd].O.C1(=CC=CC=C1)C>C[C@@H]1CCCN1CCc1cc2cc(-c3ccc(C#N)cc3)ccc2n1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-fec01abb86294747961ee324773560ef
C=CC(=O)OCC.C[C@@H]1CCCN1>>CCOC(=O)CCN1CCC[C@H]1C
Cl.C[C@H]1NCCC1.C(=O)([O-])[O-].[K+].[K+].C(C=C)(=O)OCC.CCO.C(C=C)(=O)OCC>>C(C)OC(CCN1[C@@H](CCC1)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]=[CH2:7].[NH:8]1[CH2:9][CH2:10][CH2:11][C@H:12]1[CH3:13]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH2:7][N:8]1[CH2:9][CH2:10][CH2:11][C@H:12]1[CH3:13]
C=CC(=O)OCC.C[C@@H]1CCCN1
CCOC(=O)CCN1CCC[C@H]1C
null
null
CC#N
Heteroatom Alkylation and Arylation
aza-Michael addition secondary
8e7d0268f931cff731a96db8a773eba73ff1401116a985e39d6af747cd29d378
e6898c28c2a6b7f7f5b5322689c9c6b3b6ad3dd52268b1e45ad4c4843df05f7d
C1CCNC1
[C;D1;H3:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[NH;D2;+0:6]-1.[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH;D2;+0:11]=[CH2;D1;+0:12]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH2;D2;+0:11]-[CH2;D2;+0:12]-[N;H0;D3;+0:6]1-[C:5]-[C:4]-[C:3]-[C:2]-1-[C;D1;H3:1]
100.8
[{"value": 100.8, "product": "C(C)OC(CCN1[C@@H](CCC1)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
In a round-bottom flask, 2-(R)-methylpyrrolidine HCl (5.5 g, 45 mmol) was dissolved in CH3CN (20 mL). To the stirred solution was added milled K2CO3 (8.3 g, 60 mmol). The suspension was stirred at room temperature for approximately 1 h. Ethyl acrylate (3.25 mL, 30 mmol) and EtOH (40 mL) were then added. The reaction mi...
10.6084/m9.figshare.5104873.v1
null
Ester.Secondary amine.Vinyl
Ester.Tertiary amine
C1CCNC1
C1CC[NH]C1
C1CC[NH]C1
null
CC#N
null
1
C=CC(=O)OCC.C[C@@H]1CCCN1>CC#N>CCOC(=O)CCN1CCC[C@H]1C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-ce912197d0244875aab6c2cd6dc5c11e
Nc1ccc(Br)cc1[N+](=O)[O-]>>Nc1ccc(Br)cc1N
BrC1=CC(=C(N)C=C1)[N+](=O)[O-]>>BrC=1C=C(C(=CC1)N)N
O=[N+:1]([O-])[c:2]1[cH:7][c:5]([Br:6])[cH:4][cH:3][c:8]1[NH2:9]>>[NH2:1][c:2]1[cH:3][cH:4][c:5]([Br:6])[cH:7][c:8]1[NH2:9]
Nc1ccc(Br)cc1[N+](=O)[O-]
Nc1ccc(Br)cc1N
null
[Pt]
C1CCOC1
Functional Group Interconversion
Reduction of nitro groups to amines
1613b5fba4e86adb9547d5bf6e370cff331bfa463637841d4b06138778df9f24
10b8579fd1662beac4350d758bc16e1f45ee6ea295ff9572db62110c9e2a77db
c1ccccc1
O=[N+;H0;D3:1](-[O-])-[c;H0;D3;+0:2]1:[cH;D2;+0:3]:[c:4](-[Br;D1;H0:5]):[c:6]:[cH;D2;+0:7]:[c;H0;D3;+0:8]:1-[N;D1;H2:9]>>[Br;D1;H0:5]-[c:4]1:[c:6]:[cH;D2;+0:7]:[c;H0;D3;+0:2](-[NH2;D1;+0:1]):[c;H0;D3;+0:8](-[N;D1;H2:9]):[cH;D2;+0:3]:1
103
[{"value": 103.0, "product": "BrC=1C=C(C(=CC1)N)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
4-Bromo-2-nitroaniline (12 g, 55 mmol), 1% Pt/C (1.2 g) and THF (120 mL) were added to a 250 mL bottle. The reaction mixture was hydrogenated at a pressure of approximately 40 psig H2. The hydrogenation reaction mixture was monitored by HPLC until the Area % of 4-bromo-2-nitroaniliine was less than 1%. The reaction mix...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
c1ccccc1
c1ccccc1
c1ccccc1
Other
[Pt].C1CCOC1
null
null
Nc1ccc(Br)cc1[N+](=O)[O-]>[Pt].C1CCOC1>Nc1ccc(Br)cc1N
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e1314770786e43798d6d10cde0eaf3fd
CCOC(=O)CCN1CCC[C@H]1C.Nc1ccc(Br)cc1N>>C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2[nH]1
C(C)OC(CCN1[C@@H](CCC1)C)=O.BrC=1C=C(C(=CC1)N)N.O=P12OP3(=O)OP(=O)(O1)OP(=O)(O2)O3>>BrC1=CC2=C(NC(=N2)CCN2[C@@H](CCC2)C)C=C1
CCO[C:9](=O)[CH2:8][CH2:7][N:6]1[C@H:2]([CH3:1])[CH2:3][CH2:4][CH2:5]1.[NH2:10][c:11]1[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]1[NH2:18]>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13]([Br:14])[cH:15][cH:16][c:17]2[nH:18]1
CCOC(=O)CCN1CCC[C@H]1C.Nc1ccc(Br)cc1N
C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2[nH]1
null
null
CS(=O)(=O)O
Aromatic Heterocycle Formation
OtherReaction
ae3a8ae41c7227b9865ca45cfe5b63d35f484ee7158a1d37f47008675ec00c1e
36efa24579e0043fdba8918e78f1d75cb4504837c08d344d01203f5fa64bfaef
c1ccc2[nH]c(CCN3CCCC3)nc2c1
C-C-O-[C;H0;D3;+0:1](=O)-[C:2]-[C:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[c:7](-[NH2;D1;+0:8]):[c:9]>>[C:3]-[C:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:4]:[c:5](:[c:6]):[c:7](:[c:9]):[nH;D2;+0:8]:1
40
[{"value": 40.0, "product": "BrC1=CC2=C(NC(=N2)CCN2[C@@H](CCC2)C)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
110
CELSIUS
null
null
In a round-bottom flask was charged 3-(2-(R)-methyl-pyrrolidin-1-yl)-propionic acid ethyl ester (5.6 g, 30 mmol), 4-bromo-benzene-1,2-diamine (5.6 g, 30 mmol) and 56 mL of 5% P2O5 in CH3SO3H (Eaton's reagent). After briefly stirring, the homogeneous solution was heated to 110° C. for approximately 24–48 h. The reaction...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine.Primary amine
null
c1ccccc1
c1ccc2[nH]cnc2c1
C1CC[NH]C1.c1ccc2[nH]cnc2c1
HO-
CS(=O)(=O)O
110
null
CCOC(=O)CCN1CCC[C@H]1C.Nc1ccc(Br)cc1N>CS(=O)(=O)O>C[C@@H]1CCCN1CCc1nc2cc(Br)ccc2[nH]1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-14f696dcbf5a4434a0b46e260bb5ebf6
CC1CCCN1CCc1nc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1>>C[C@@H]1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
C(=O)([O-])[O-].[Na+].[Na+].BrC1=CC2=C(NC(=N2)CCN2C(CCC2)C)C=C1.C(#N)C1=CC=C(C=C1)B(O)O>>C[C@H]1N(CCC1)CCC1=NC2=C(N1)C=CC(=C2)C2=CC=C(C#N)C=C2
Br[c:13]1[cH:12][c:11]2[n:10][c:9]([CH2:8][CH2:7][N:6]3[CH:2]([CH3:1])[CH2:3][CH2:4][CH2:5]3)[nH:25][c:24]2[cH:23][cH:22]1.OB(O)[c:14]1[cH:15][cH:16][c:17]([C:18]#[N:19])[cH:20][cH:21]1>>[CH3:1][C@@H:2]1[CH2:3][CH2:4][CH2:5][N:6]1[CH2:7][CH2:8][c:9]1[n:10][c:11]2[cH:12][c:13](-[c:14]3[cH:15][cH:16][c:17]([C:18]#[N:19])...
CC1CCCN1CCc1nc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1
C[C@@H]1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
null
C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].C(Cl)Cl
O.COCCOC
C-C Coupling
Suzuki coupling with boronic acids
4c01b75ced48e0c5dbfbda4cb6a596e9d3a1d181f4aef3fbd9604232ef2322c4
08d2969413ef1a2cd5b43667268ba178160c7b55545bf48018e31f2b019632ec
c1ccc(-c2ccc3[nH]c(CCN4CCCC4)nc3c2)cc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:2:[c:8]:[c:9]:1.O-B(-O)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14]>>[c:12]:[c:11]:[c;H0;D3;+0:10](-[c;H0;D3;+0:1]1:[c:2]:[c:3]2:[#7;a:4]:[c:5]:[#7;a:6]:[c:7]:2:[c:8]:[c:9]:1):[c:13]:[c:14]
40.4
[{"value": 40.4, "product": "C[C@H]1N(CCC1)CCC1=NC2=C(N1)C=CC(=C2)C2=CC=C(C#N)C=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
24
HOUR
Nitrogen (N2) gas was bubbled through a solution of 5-bromo-2-[2-(2-methyl-pyrrolidin-1-yl)-ethyl]-1H-benzoimidazole (0.19 g, 0.6 mmol) and 4-cyanophenylboronic acid (0.13 g, 0.9 mmol) in 1,2-dimethoxyethane (4 mL) and H2O (2 mL). To the mixture was added 2M Na2CO3 (1.2 mL, 2.4 mmol) and Pd(dppf)2Cl2:CH2Cl2 (1:1), and ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Boronic acid
null
c1ccc2[nH]cnc2c1.c1ccccc1
c1ccc2[nH]cnc2c1.c1ccccc1
C1CC[NH]C1.c1ccc2[nH]cnc2c1.c1ccccc1
HBr.B
C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].C(Cl)Cl.O.COCCOC
80
24
CC1CCCN1CCc1nc2cc(Br)ccc2[nH]1.N#Cc1ccc(B(O)O)cc1>C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.C1=CC=C(C=C1)P([C-]2C=CC=C2)C3=CC=CC=C3.Cl[Pd]Cl.[Fe+2].C(Cl)Cl.O.COCCOC>C[C@@H]1CCCN1CCc1nc2cc(-c3ccc(C#N)cc3)ccc2[nH]1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-d12afd9173344f0ea591ca507c1e1ff0
CC(=O)OC(C)(C)C.O=C1CC[C@@H](C(=O)O)N1>>CC(C)(C)OC(=O)[C@@H]1CCC(=O)N1
C(C)(=O)OC(C)(C)C.N1[C@@H](CCC1=O)C(=O)O.Cl(=O)(=O)(=O)O.[OH-].[Na+]>>O=C1CC[C@H](N1)C(=O)OC(C)(C)C
CC(=O)[O:5][C:2]([CH3:1])([CH3:3])[CH3:4].O[C:6](=[O:7])[C@@H:8]1[CH2:9][CH2:10][C:11](=[O:12])[NH:13]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@@H:8]1[CH2:9][CH2:10][C:11](=[O:12])[NH:13]1
CC(=O)OC(C)(C)C.O=C1CC[C@@H](C(=O)O)N1
CC(C)(C)OC(=O)[C@@H]1CCC(=O)N1
null
null
O
Acylation
OtherReaction
5eda8161d36467b4dc537f76ab93cf348d82102ac40d865b5fccff23d019462d
03baa9d39762bbc48d7dd927c5c80fc17976a560c4f5aa44c95e8b810d3c70c8
O=C1CCCN1
C-C(=O)-[O;H0;D2;+0:1]-[C:2](-[C;D1;H3:3])(-[C;D1;H3:4])-[C;D1;H3:5].O-[C;H0;D3;+0:6](=[O;D1;H0:7])-[C:8](-[C:9])-[#7:10]-[C:11]=[O;D1;H0:12]>>[C:9]-[C:8](-[C;H0;D3;+0:6](=[O;D1;H0:7])-[O;H0;D2;+0:1]-[C:2](-[C;D1;H3:3])(-[C;D1;H3:4])-[C;D1;H3:5])-[#7:10]-[C:11]=[O;D1;H0:12]
null
[]
null
null
12
HOUR
129 g of L-pyroglutamic acid were suspended in 2 l of tert-butyl acetate. 30 ml of a 70% strength solution of perchloric acid in water were added thereto. The mixture was then stirred at room temperature for 12 h. It was cooled to 0° C. and the pH of the solution was adjusted to 7 by cautious addition of a 2N NaOH solu...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester
Ester
null
null
C1CCNC1
HO-
O
null
12
CC(=O)OC(C)(C)C.O=C1CC[C@@H](C(=O)O)N1>O>CC(C)(C)OC(=O)[C@@H]1CCC(=O)N1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-36ba26068fa844f5b119a23fefe3f5e6
CC(C)(C)OC(=O)[C@@H]1CCC(=O)N1C(=O)OC(C)(C)C>>CC(C)(C)OC(=O)[C@@H]1CCC(O)N1C(=O)OC(C)(C)C
C([O-])(O)=O.[Na+].C(C)[BH-](CC)CC.[Li+].O=C1CC[C@H](N1C(=O)OC(C)(C)C)C(=O)OC(C)(C)C.OO>>OC1CC[C@H](N1C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@@H:8]1[CH2:9][CH2:10][C:11](=[O:12])[N:13]1[C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@@H:8]1[CH2:9][CH2:10][CH:11]([OH:12])[N:13]1[C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20]
CC(C)(C)OC(=O)[C@@H]1CCC(=O)N1C(=O)OC(C)(C)C
CC(C)(C)OC(=O)[C@@H]1CCC(O)N1C(=O)OC(C)(C)C
null
null
C1CCOC1
Reduction
OtherReaction
7a66ad41b54bb485918a759dc010bded0c65a7503d10eee13c33ae0017305eee
6c2222fa5333790df8c936ae3761255cb080c6e237292637f62137781815b926
C1CCNC1
[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]1-[C:5]-[C:6]-[C;H0;D3;+0:7](=[O;H0;D1;+0:8])-[#7:9]-1-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13](-[C;D1;H3:14])(-[C;D1;H3:15])-[C;D1;H3:16]>>[#8:1]-[C:2](=[O;D1;H0:3])-[C:4]1-[C:5]-[C:6]-[CH;D3;+0:7](-[OH;D1;+0:8])-[#7:9]-1-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13](-[C;D1;H3:14])(-[C;D1;H3:15])-[C...
null
[]
-78
CELSIUS
30
MINUTE
93 g of di-tert-butyl (S)-5-oxopyrrolidine-1,2-dicarboxylate were dissolved in 600 ml of THF and cooled to −78° C. 392 ml of a 1N solution of lithium triethylborohydride in THF were added dropwise over the course of 90 min. The mixture was then stirred at −70° C. for 30 min. Subsequently, 240 ml of saturated sodium bic...
10.6084/m9.figshare.5104873.v1
null
Substituted dicarboximide
Secondary alcohol
C1CC[NH]C1
C1CC[NH]C1
C1CC[NH]C1
null
C1CCOC1
-78
0.5
CC(C)(C)OC(=O)[C@@H]1CCC(=O)N1C(=O)OC(C)(C)C>C1CCOC1>CC(C)(C)OC(=O)[C@@H]1CCC(O)N1C(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-2ee3358ec00f4d3a99109190e3ee13ea
CCOC(=O)C[C@@H]1CC[C@@H](C(=O)OC(C)(C)C)N1C(=O)OC(C)(C)C>>CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CCO)N1C(=O)OC(C)(C)C
C([O-])(O)=O.[K+].C(C)OC(=O)C[C@@H]1CC[C@H](N1C(=O)OC(C)(C)C)C(=O)OC(C)(C)C.[BH4-].[Li+]>>OCC[C@@H]1CC[C@H](N1C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
CCO[C:13]([CH2:12][C@@H:11]1[CH2:10][CH2:9][C@@H:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[N:15]1[C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:14]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@@H:8]1[CH2:9][CH2:10][C@@H:11]([CH2:12][CH2:13][OH:14])[N:15]1[C:16](=[O:17])[O:18][C:19]([CH3:2...
CCOC(=O)C[C@@H]1CC[C@@H](C(=O)OC(C)(C)C)N1C(=O)OC(C)(C)C
CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CCO)N1C(=O)OC(C)(C)C
null
null
C(C)OCC
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
C1CCNC1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3]-[C:4]-[#7:5]>>[#7:5]-[C:4]-[C:3]-[CH2;D2;+0:1]-[OH;D1;+0:2]
null
[]
null
null
6
HOUR
43 g of the product from 1d were dissolved in 300 ml of diethyl ether. A solution of 3.1 g of lithium borohydride in 300 ml of diethyl ether was added dropwise thereto. The mixture was stirred for 6 h and the reaction was stopped by cautious addition of 300 ml of a saturated potassium bicarbonate solution. The phases w...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
C1CC[NH]C1
HO-
C(C)OCC
null
6
CCOC(=O)C[C@@H]1CC[C@@H](C(=O)OC(C)(C)C)N1C(=O)OC(C)(C)C>C(C)OCC>CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CCO)N1C(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-eec8fdcdd0e0440fb1b9c9b1ae69362f
CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(C#N)NCc2ccccc2)N1C(=O)OC(C)(C)C.OO>>CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(NCc2ccccc2)C(N)=O)N1C(=O)OC(C)(C)C
C(C1=CC=CC=C1)NC(C[C@@H]1CC[C@H](N1C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C#N.C([O-])([O-])=O.[K+].[K+].OO>>C(C1=CC=CC=C1)NC(C[C@@H]1CC[C@H](N1C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C(N)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@@H:8]1[CH2:9][CH2:10][C@@H:11]([CH2:12][CH:13]([NH:14][CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[C:22]#[N:23])[N:25]1[C:26](=[O:27])[O:28][C:29]([CH3:30])([CH3:31])[CH3:32].O[OH:24]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[C@@H:8]1[CH2:9][CH2:10][C@@...
CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(C#N)NCc2ccccc2)N1C(=O)OC(C)(C)C.OO
CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(NCc2ccccc2)C(N)=O)N1C(=O)OC(C)(C)C
null
null
CS(=O)C.O
Heteroatom Alkylation and Arylation
Nitrile and hydrogen peroxide to amide
b438c1a5a5f49012c6adf1e24ab44bc669089beaf4e5b0289cbfa931d3ceafda
37ed9176b981633816a0414a3f5b39ee33c11d757fe87a2cac8fe30b523bffdf
c1ccc(CNCC[C@@H]2CCCN2)cc1
O-[OH;D1;+0:1].[#7:2]-[C:3](-[C:4])-[C;H0;D2;+0:5]#[N;H0;D1;+0:6]>>[#7:2]-[C:3](-[C:4])-[C;H0;D3;+0:5](-[NH2;D1;+0:6])=[O;H0;D1;+0:1]
null
[]
null
null
14
HOUR
2.6 g of di-tert-butyl (2S,5S)-5-(2-benzylamino-2-cyanoethyl)pyrrolidine-1,2-dicarboxylate were dissolved in 6.5 ml of dimethyl sulfoxide. 373 mg of finely ground potassium carbonate and 1.08 ml of a 30% strength hydrogen peroxide solution were added thereto. The mixture was stirred at room temperature for 14 h and was...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Peroxide
Primary amide
null
null
C1CC[NH]C1.c1ccccc1
Other
CS(=O)C.O
null
14
CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(C#N)NCc2ccccc2)N1C(=O)OC(C)(C)C.OO>CS(=O)C.O>CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(NCc2ccccc2)C(N)=O)N1C(=O)OC(C)(C)C
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e2f54db65abf48f99044f31ef5758d3e
CC(=O)O.CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(NCc2ccccc2)C(N)=O)N1C(=O)OC(C)(C)C>>CC(C)(C)OC(=O)N1[C@H](CC(NCc2ccccc2)C(=O)O)CC[C@H]1C(=O)O
C(C)(=O)O.[OH-].[Na+].C(C1=CC=CC=C1)NC(C[C@@H]1CC[C@H](N1C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C(N)=O>>C(C)(C)(C)OC(=O)N1[C@@H](CC[C@H]1CC(C(=O)O)NCC1=CC=CC=C1)C(=O)O
CC(=O)[OH:22].CC(C)(C)[O:28][C:26]([C@H:25]1[N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[C@H:9]([CH2:10][CH:11]([NH:12][CH2:13][c:14]2[cH:15][cH:16][cH:17][cH:18][cH:19]2)[C:20](N)=[O:21])[CH2:23][CH2:24]1)=[O:27]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[C@H:9]([CH2:10][CH:11]([NH:12][CH2:13][...
CC(=O)O.CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(NCc2ccccc2)C(N)=O)N1C(=O)OC(C)(C)C
CC(C)(C)OC(=O)N1[C@H](CC(NCc2ccccc2)C(=O)O)CC[C@H]1C(=O)O
null
null
O.C(C)O
Acylation
OtherReaction
c189ddade6f073abd1f049c2ff7589d7ef3c92298598276005c6db1a5bca9bfe
921dee6249f084a5afe68b361e3119014cbca8bae41456f33247d587f86f399e
c1ccc(CNCC[C@@H]2CCCN2)cc1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[#7:5].N-[C;H0;D3;+0:6](=[O;D1;H0:7])-[C:8](-[#7:9])-[C:10].C-C(=O)-[OH;D1;+0:11]>>[#7:9]-[C:8](-[C:10])-[C;H0;D3;+0:6](=[O;D1;H0:7])-[OH;D1;+0:11].[#7:5]-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
null
[]
null
null
null
null
2.2 g of di-tert-butyl (2S,5S)-5-(2-benzylamino-2-carbamoylethyl)pyrrolidine-1,2-dicarboxylate were dissolved in 20 ml of ethanol and 5 ml of water. 1.2 g of solid sodium hydroxide were added thereto. The solution was then boiled under reflux for 36 h. For workup, it was cooled to room temperature and neutralized with ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester.Primary amide.Boc
Carboxylic acid.Carboxylic acid
null
null
C1CC[NH]C1.c1ccccc1
HO-
O.C(C)O
null
null
CC(=O)O.CC(C)(C)OC(=O)[C@@H]1CC[C@@H](CC(NCc2ccccc2)C(N)=O)N1C(=O)OC(C)(C)C>O.C(C)O>CC(C)(C)OC(=O)N1[C@H](CC(NCc2ccccc2)C(=O)O)CC[C@H]1C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0671b17e79594082bfe04925787d737d
CC(C)(C)OC(=O)N1[C@H](CC(NCc2ccccc2)C(=O)O)CC[C@H]1C(=O)O>>CC(=O)O.CC(C)(C)OC(=O)N1[C@H](CC(N)C(=O)O)CC[C@H]1C(=O)O
C(C)(C)(C)OC(=O)N1[C@@H](CC[C@H]1CC(C(=O)O)NCC1=CC=CC=C1)C(=O)O.[H][H]>>C(C)(=O)O.C(C)(C)(C)OC(=O)N1[C@@H](CC[C@H]1CC(C(=O)O)N)C(=O)O
c1cc(C[NH:16][CH:15]([CH2:14][C@H:13]2[N:12]([C:10]([O:9][C:6]([CH3:5])([CH3:7])[CH3:8])=[O:11])[C@H:22]([C:23](=[O:24])[OH:25])[CH2:21][CH2:20]2)[C:17](=[O:3])[OH:19])[cH:2][cH:1]c1>>[CH3:1][C:2](=[O:3])[OH:4].[CH3:5][C:6]([CH3:7])([CH3:8])[O:9][C:10](=[O:11])[N:12]1[C@H:13]([CH2:14][CH:15]([NH2:16])[C:17](=[O:18])[OH...
CC(C)(C)OC(=O)N1[C@H](CC(NCc2ccccc2)C(=O)O)CC[C@H]1C(=O)O
CC(=O)O.CC(C)(C)OC(=O)N1[C@H](CC(N)C(=O)O)CC[C@H]1C(=O)O
null
[OH-].[OH-].[Pd+2]
C(C)(=O)O
Functional Group Addition
OtherReaction
7c943473f923398f2f254efe37c2a78ee586499f5f8405c367aad51e852a90f9
e966341af73f102bbef49d8ca706ff70a257f9f835ed69f2c7c4cc33532963a2
C1CCNC1
[C:1]-[C:2](-[NH;D2;+0:3]-C-c1:[cH;D2;+0:4]:[cH;D2;+0:5]:c:c:c:1)-[C;H0;D3;+0:6](-[O;D1;H1:7])=[O;H0;D1;+0:8]>>[CH3;D1;+0:5]-[C;H0;D3;+0:4](-[O;D1;H1:9])=[O;H0;D1;+0:8].[C:1]-[C:2](-[NH2;D1;+0:3])-[C;H0;D3;+0:6](=[O;D1;H0:10])-[O;D1;H1:7]
null
[]
null
null
10
MINUTE
1600 mg of (2S,5S)-5-(2-benzylamino-2-carboxyethyl)pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester were dissolved in 30 ml of acetic acid. 100 mg of 20% palladium hydroxide on activated carbon were added thereto, and the mixture was hydrogenated under an atmosphere of 1 bar of hydrogen for 1 h. Ar was then passed ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amine
Carboxylic acid.Carboxylic acid.Primary amine
c1ccccc1
null
C1CC[NH]C1
Other
[OH-].[OH-].[Pd+2].C(C)(=O)O
null
0.166667
CC(C)(C)OC(=O)N1[C@H](CC(NCc2ccccc2)C(=O)O)CC[C@H]1C(=O)O>[OH-].[OH-].[Pd+2].C(C)(=O)O>CC(=O)O.CC(C)(C)OC(=O)N1[C@H](CC(N)C(=O)O)CC[C@H]1C(=O)O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-cb72a94ce0d34f9d96a25ac130802067
COC(=O)C(C[C@@H]1CC[C@@H](C(=O)OC)N1C(=O)OC(C)(C)C)NC(=O)OCc1ccccc1>>COC(=O)[C@@H]1CC[C@H]2CC(NC(=O)OCc3ccccc3)C(=O)N21
C(C1=CC=CC=C1)OC(=O)NC(C[C@@H]1CC[C@H](N1C(=O)OC(C)(C)C)C(=O)OC)C(=O)OC.C1(=CC=CC=C1)SC>>C(C1=CC=CC=C1)OC(=O)NC1C(N2[C@@H](CC[C@H]2C1)C(=O)OC)=O
CO[C:22]([CH:10]([CH2:9][C@@H:8]1[CH2:7][CH2:6][C@@H:5]([C:3]([O:2][CH3:1])=[O:4])[N:24]1C(=O)OC(C)(C)C)[NH:11][C:12](=[O:13])[O:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1)=[O:23]>>[CH3:1][O:2][C:3](=[O:4])[C@@H:5]1[CH2:6][CH2:7][C@H:8]2[CH2:9][CH:10]([NH:11][C:12](=[O:13])[O:14][CH2:15][c:16]3[cH:17][cH:18...
COC(=O)C(C[C@@H]1CC[C@@H](C(=O)OC)N1C(=O)OC(C)(C)C)NC(=O)OCc1ccccc1
COC(=O)[C@@H]1CC[C@H]2CC(NC(=O)OCc3ccccc3)C(=O)N21
null
null
FC(C(=O)O)(F)F
Miscellaneous
OtherReaction
4418e988074acea71dd24ac14a7ea7a4f3d5446e60376f467c44f429251f5664
68b3dbac8e61dda6bb0cc2ed5a0f03fe36b9f9015e9dcb1e6046c632f9edd41f
O=C(NC1C[C@@H]2CCCN2C1=O)OCc1ccccc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[#7:4]-[C:5]=[O;D1;H0:6])-[C:7]-[C:8]1-[C:9]-[C:10]-[C:11](-[C:12](=[O;D1;H0:13])-[#8:14]-[C;D1;H3:15])-[N;H0;D3;+0:16]-1-C(=O)-O-C(-C)(-C)-C>>[C;D1;H3:15]-[#8:14]-[C:12](=[O;D1;H0:13])-[C:11]1-[C:10]-[C:9]-[C:8]2-[C:7]-[C:3](-[#7:4]-[C:5]=[O;D1;H0:6])-[C;H0;D3;+0:1](=[O;D1;H0:2]...
null
[]
95
CELSIUS
45
MINUTE
1500 mg of 1-tert-butyl 2-methyl (2S,5S)-5-(2-benzyloxycarbonylamino-2-methoxycarbonylethyl)pyrrolidine-1,2-dicarboxylate were mixed with 0.2 ml of thioanisole. Then 10 ml of trifluoroacetic acid were added, and the mixture was stirred for 45 min. The solvents were then removed in vacuo, and the residue was taken up in...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ester.Ether.Boc
Tertiary amide
C1CC[NH]C1
C1CC2CCCN2C1
C1CC2CCCN2C1.c1ccccc1
HO-
FC(C(=O)O)(F)F
95
0.75
COC(=O)C(C[C@@H]1CC[C@@H](C(=O)OC)N1C(=O)OC(C)(C)C)NC(=O)OCc1ccccc1>FC(C(=O)O)(F)F>COC(=O)[C@@H]1CC[C@H]2CC(NC(=O)OCc3ccccc3)C(=O)N21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-93eff2bf0daa450c897e724582f37625
CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C(N)=O)N2C1=O>>CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C#N)N2C1=O
C(N)(=O)[C@H]1N2C([C@@H](C[C@@H]2CC1)NC(OC(C)(C)C)=O)=O.N1=C(Cl)N=C(Cl)N=C1Cl>>C(#N)[C@H]1N2C([C@@H](C[C@@H]2CC1)NC(OC(C)(C)C)=O)=O
O=[C:15]([C@@H:14]1[CH2:13][CH2:12][C@H:11]2[CH2:10][C@@H:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[C:18](=[O:19])[N:17]21)[NH2:16]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][C@@H:9]1[CH2:10][C@@H:11]2[CH2:12][CH2:13][C@@H:14]([C:15]#[N:16])[N:17]2[C:18]1=[O:19]
CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C(N)=O)N2C1=O
CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C#N)N2C1=O
null
null
CN(C=O)C
Miscellaneous
OtherReaction
5094e9d814705bbdc421edbf7e9198e499e70e93916e2cec6eefbc82d1ba5440
32b9893bcb5223559a9d02852f8392cf6473aacfb044a52ba4e9cb9c29edb170
O=C1CC[C@@H]2CCCN12
O=[C;H0;D3;+0:1](-[NH2;D1;+0:2])-[C:3](-[C:4])-[#7:5](-[C:6])-[C:7]=[O;D1;H0:8]>>[C:6]-[#7:5](-[C:7]=[O;D1;H0:8])-[C:3](-[C;H0;D2;+0:1]#[N;H0;D1;+0:2])-[C:4]
null
[]
null
null
3
HOUR
100 mg of tert-butyl ((2R,5S,7aS)-5-carbamoyl-3-oxohexahydropyrrolizin-2-yl)carbamate were dissolved in 2 ml of dimethylformamide, and 65 mg of cyanuric chloride were added. The mixture was stirred for 3 h, and the dimethylformamide was removed in vacuo. The residue was chromatographed on silica gel. Conditions: See re...
10.6084/m9.figshare.5104873.v1
null
Primary amide
Nitrile
null
null
C1CC2CCCN2C1
HO-
CN(C=O)C
null
3
CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C(N)=O)N2C1=O>CN(C=O)C>CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C#N)N2C1=O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-300496268f1a4ca7a2622d242dab1799
CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C#N)N2C1=O>>N#C[C@@H]1CC[C@H]2C[C@@H](N)C(=O)N21
C(#N)[C@H]1N2C([C@@H](C[C@@H]2CC1)NC(OC(C)(C)C)=O)=O.C1(=CC=CC=C1)SC.FC(C(=O)O)(F)F>>FC(C(=O)O)(F)F.N[C@H]1C(N2[C@@H](CC[C@H]2C1)C#N)=O
CC(C)(C)OC(=O)[NH:9][C@@H:8]1[CH2:7][C@@H:6]2[CH2:5][CH2:4][C@@H:3]([C:2]#[N:1])[N:12]2[C:10]1=[O:11]>>[N:1]#[C:2][C@@H:3]1[CH2:4][CH2:5][C@H:6]2[CH2:7][C@@H:8]([NH2:9])[C:10](=[O:11])[N:12]12
CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C#N)N2C1=O
N#C[C@@H]1CC[C@H]2C[C@@H](N)C(=O)N21
null
null
null
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
O=C1CC[C@@H]2CCCN12
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]1-[C:3]-[C:4]-[#7:5](-[C:6])-[C:7]-1=[O;D1;H0:8]>>[C:6]-[#7:5]1-[C:4]-[C:3]-[C:2](-[NH2;D1;+0:1])-[C:7]-1=[O;D1;H0:8]
null
[]
null
null
null
null
80 mg of tert-butyl ((2R,5S,7aS)-5-cyano-3-oxohexahydropyrrolizin-2-yl)carbamate were C reacted with 10% thioanisole in 1 ml of trifluoroacetic acid for 30 min. The solvents were then removed in vacuo, and the residue was stirred with diusopropyl ether. Conditions: See reaction.notes.procedure_details. Workup: The solv...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
C1CC2CCCN2C1
HO-
null
null
null
CC(C)(C)OC(=O)N[C@@H]1C[C@@H]2CC[C@@H](C#N)N2C1=O>>N#C[C@@H]1CC[C@H]2C[C@@H](N)C(=O)N21
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c9095f644eb14828b9bed161b97caec1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O.O=C(NCCN1CCCCC1)n1ccnc1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN4CCCCC4)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(CCCCC1)CCNC(=O)N1C=NC=C1.C1(=CC=CC=C1)C.C(C)(C)O.N1(CCCCC1)CCNC(=O)N1C=NC=C1>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NCCN1CCCCC1)[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:48][c:49]23)[C@H:50]([OH:51])[C@@H:52]1[OH:53].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(NCCN1CCCCC1)n1ccnc1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN4CCCCC4)nc32)[C@H](O)[C@@H]1O
null
null
ClCCl
Acylation
OtherReaction
2fca1e60b30bb25dd42d9c3a0a409c10e22201738c1a0d1497c17610c9a7f90b
11d83d172c98dee16e5582fbe84e86af1814ed957a762275a38224e82e89f00a
O=C(NCCNC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@H]3CCCO3)c2n1)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:5]-[C:6]-[NH;D2;+0:7]-[C;H0;D3;+0:3](=[O;D1;H0:4])-[#7:2]-[C:1]
54.9
[{"value": 54.9, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NCCN1CCCCC1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
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) (90 mg, 0.15 mmol) and N-[2-(1-piperidinyl)ethyl]-1H-imidazole-1-carboxamide (Preparation 18) (36 mg, 0.16 mmol) were dissolved in dichloromethane (3 ml). ...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Primary amine
Urea
c1c[nH]cn1
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CC[NH]CC1
Other
ClCCl
null
4
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O.O=C(NCCN1CCCCC1)n1ccnc1>ClCCl>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN4CCCCC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-69c7055820c24dc2be3109de07647118
CC(C)C1CCN(CCNC(=O)n2ccnc2)CC1.CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN4CCC(C(C)C)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.C(C)(C)C1CCN(CC1)CCNC(=O)N1C=NC=C1>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NCCN1CCC(CC1)C(C)C)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1
c1cn([C:37](=[O:38])[NH:39][CH2:40][CH2:41][N:42]2[CH2:43][CH2:44][CH:45]([CH:46]([CH3:47])[CH3:48])[CH2:49][CH2:50]2)cn1.[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...
CC(C)C1CCN(CCNC(=O)n2ccnc2)CC1.CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN4CCC(C(C)C)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)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: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 N-[2-(4-isopropyl-1-piperidinyl)ethyl]-1H-imidazole-1-carboxamide (Preparation 22) by a similar method to Example 1. Conditions: See react...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Primary amine
Urea
c1c[nH]cn1
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CC[NH]CC1
Other
null
null
null
CC(C)C1CCN(CCNC(=O)n2ccnc2)CC1.CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN4CCC(C(C)C)CC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-59ce50b918274a759994faec492ad9c0
CC(C)N(CCNC(=O)n1ccnc1)C1CCCC1.CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN(C(C)C)C4CCCC4)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.C1(CCCC1)N(CCNC(=O)N1C=NC=C1)C(C)C>>C1(CCCC1)N(CCNC(=O)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)C(C)C
c1cn([C:37](=[O:38])[NH:39][CH2:40][CH2:41][N:42]([CH:43]([CH3:44])[CH3:45])[CH:46]2[CH2:47][CH2:48][CH2:49][CH2:50]2)cn1.[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...
CC(C)N(CCNC(=O)n1ccnc1)C1CCCC1.CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN(C(C)C)C4CCCC4)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)NCCNC1CCCC1
[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 N-{2-[cyclopentyl(isopropyl)amino]ethyl}-1H-imidazole-1-carboxamide (Preparation 26) by a similar method to Example 1. Conditions: See rea...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Primary amine
Urea
c1c[nH]cn1
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CCCC1
Other
null
null
null
CC(C)N(CCNC(=O)n1ccnc1)C1CCCC1.CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCCN(C(C)C)C4CCCC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-e37cd6d45bd145b4bd9f02d588d506a7
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O.O=C(NC1CCN(c2ccccn2)CC1)n1ccnc1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)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(C=CC=C1)N1CCC(CC1)NC(=O)N1C=NC=C1>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NC1CCN(CC1)C1=NC=CC=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:52][c:53]23)[C@H:54]([OH:55])[C@@H:56]1[OH:57].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(NC1CCN(c2ccccn2)CC1)n1ccnc1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)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)NC1CCN(c2ccccn2)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 N-[1-(2-pyridinyl)-4-piperidinyl]-1H-imidazole-1-carboxamide (Preparation 30) by a similar method to Example 1. Conditions: See reaction.n...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Primary amine
Urea
c1c[nH]cn1
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CC[NH]CC1.c1ccncc1
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(NC1CCN(c2ccccn2)CC1)n1ccnc1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)CC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-7fde1ea0769641d099aecaf4a6f8b926
CC(C)N(CCNC(=O)NCCN)C(C)C.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>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4cccc(C)c4)c4cccc(C)c4)nc(C(=O)NCCNC(=O)NCCN(C(C)C)C(C)C)nc32)[C@H](O)[C@@H]1O
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.NCCNC(=O)NCCN(C(C)C)C(C)C.C1CCOC1>>CC=1C=C(C=CC1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NCCN(C(C)C)C(C)C)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC(=CC=C1)C
[NH2:35][CH2:36][CH2:37][NH:38][C:39](=[O:40])[NH:41][CH2:42][CH2:43][N:44]([CH:45]([CH3:46])[CH3:47])[CH:48]([CH3:49])[CH3:50].O=C(c1ccccc1)[O:56][C@@H:55]1[C@@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[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][c:21]([CH3:22])[cH:23...
CC(C)N(CCNC(=O)NCCN)C(C)C.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
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4cccc(C)c4)c4cccc(C)c4)nc(C(=O)NCCNC(=O)NCCN(C(C)C)C(C)C)nc32)[C@H](O)[C@@H]1O
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
null
Acylation
OtherReaction
2ae826299acf86d14128c62181c55ea7931ee4517720883c75fc6ce1f929a22c
c9ac21fd27fbb51e10283d4cb3296223e3218179c867ce8e9d01fd6be8878238
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
I-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]2:[#7;a:5]:[c:6]:[#7;a:7](-[C:8]3-[#8:9]-[C:10](-[C:11](-[#7:12])=[O;D1;H0:13])-[C:14](-[O;H0;D2;+0:15]-C(=O)-c4:c:c:c:c:c:4)-[C:16]-3-[O;H0;D2;+0:17]-[C;H0;D3;+0:18](=[O;D1;H0:19])-c3:c:c:c:c:c:3):[c:20]:2:[#7;a:21]:1.[C:22]-[C:23]-[NH2;D1;+0:24]>>[#7:12]-[C:11](=[O;D1;H0:13])-[C:...
null
[]
null
null
14
HOUR
A solution of (2R,3R,4S,5S)-4-(benzoyloxy)-2-(6-{[2,2-bis(3-methylphenyl)ethyl]amino}-2-iodo-9H-purin-9-yl)-5-[(ethylamino)carbonyl]tetrahydro-3-furanyl benzoate (Preparation 48) (200 mg, 0.24 mmol), N-(2-aminoethyl)-N′-[2-(diisopropylamino)ethyl]urea (Preparation 52) (270 mg, 1.18 mmol) and tetrakis(triphenylphosphine...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ester.Ester.Primary amine
Secondary amide.Secondary alcohol.Secondary alcohol
c1ccccc1.c1ncc2nc[nH]c2n1.c1ccccc1
c1ncc2nc[nH]c2n1
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1
HI
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
null
14
CC(C)N(CCNC(=O)NCCN)C(C)C.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=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>CCNC(=O)[C@H...
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-b3667a2bae3747a0957314fe0b87f185
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>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCc4ccc(C(=O)O)cc4)nc32)[C@H](O)[C@@H]1O
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>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NCC1=CC=C(C(=O)O)C=C1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1
c1ccc(C[O:47][C:45]([c:44]2[cH:43][cH:42][c:41]([CH2:40][NH:39][C:37]([NH:36][CH2:35][CH2:34][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])...
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
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCc4ccc(C(=O)O)cc4)nc32)[C@H](O)[C@@H]1O
null
[Pd]
C(C)O
Deprotection
Ester saponification (alkyl deprotection)
86a971d3e4f88009ab4c98512e9f1deb51b2f0ce5cbd068cc61ae878c1e58e2a
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C(NCCNC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@H]3CCCO3)c2n1)NCc1ccccc1
[O;D1;H0:1]=[C:2](-[c:3])-[O;H0;D2;+0:4]-C-c1:c:c:c:c:c:1>>[O;D1;H0:1]=[C:2](-[OH;D1;+0:4])-[c:3]
19.2
[{"value": 19.2, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NCC1=CC=C(C(=O)O)C=C1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of benzyl 4-[({[(2-{[(6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purin-2-yl)carbonyl]amino}ethyl)amino]carbonyl}amino)methyl]benzoate (Preparation 55) (150 mg, 0.18 mmol) in ethanol (10 ml) was hydrogenated at room temperature over 10% w/w pal...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
c1ccccc1
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.c1ccccc1
Other
[Pd].C(C)O
null
null
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>[Pd].C(C)O>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NCc4ccc(C(=O)O)cc4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-4737901165ba46a4813fc2f285affa0e
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)CC4)nc32)[C@@H]2OC(C)(C)O[C@@H]21>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)CC4)nc32)[C@H](O)[C@@H]1O
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)NCCNC(=O)NC2CCN(CC2)C2=NC=CC=C2.Cl.C([O-])(O)=O.[Na+]>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C(=O)NCCNC(=O)NC1CCN(CC1)C1=NC=CC=C1)[C@@H]1O[C@@H]([C@H]([C@H]1O)O)C(=O)NCC)C1=CC=CC=C1
CC1(C)[O:55][C@H:54]2[C@H:8]([n:9]3[cH:10][n:11][c:12]4[c:13]([NH:14][CH2:15][CH:16]([c:17]5[cH:18][cH:19][cH:20][cH:21][cH:22]5)[c:23]5[cH:24][cH:25][cH:26][cH:27][cH:28]5)[n:29][c:30]([C:31](=[O:32])[NH:33][CH2:34][CH2:35][NH:36][C:37](=[O:38])[NH:39][CH:40]5[CH2:41][CH2:42][N:43]([c:44]6[cH:45][cH:46][cH:47][cH:48][...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)CC4)nc32)[C@@H]2OC(C)(C)O[C@@H]21
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)CC4)nc32)[C@H](O)[C@@H]1O
null
null
C(C)O
Deprotection
Acetal hydrolysis to diol
cd7d99316c4d16a7c810595d0c5705cc11ed3a94563ee4b1b511c64a517d01aa
3cb0396ca8ad36859ee8d51a67a558871ec1b96bb69d5cbac40dafd7041336b3
O=C(NCCNC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn([C@H]3CCCO3)c2n1)NC1CCN(c2ccccn2)CC1
C-C1(-C)-[O;H0;D2;+0:1]-[C:2]2-[C:3]-[#8:4]-[C:5](-[C:6](-[#7:7])=[O;D1;H0:8])-[C:9]-2-[O;H0;D2;+0:10]-1>>[#7:7]-[C:6](=[O;D1;H0:8])-[C:5]1-[#8:4]-[C:3]-[C:2](-[OH;D1;+0:1])-[C:9]-1-[OH;D1;+0:10]
null
[]
null
null
null
null
To a solution of 9-{(3aR,4R,6S,6aS)-6-[(ethylamino)carbonyl]-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl}-6-[(2,2-diphenylethyl)amino]-N-{2-[({[1-(2-pyridinyl)-4-piperidinyl]amino}carbonyl)amino]ethyl}-9H-purine-2-carboxamide (Preparation 71) (20.9 g, 0.0255 moles) in absolute ethanol (200 ml) was added aqueous h...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Secondary alcohol.Secondary alcohol
C1O[C@H]2COC[C@H]2O1
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1.C1CC[NH]CC1.c1ccncc1
Other
C(C)O
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)CC4)nc32)[C@@H]2OC(C)(C)O[C@@H]21>C(C)O>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCNC(=O)NC4CCN(c5ccccn5)CC4)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-69e4a8157db7424a83d31d8e7356ee4a
C1=COCCC1.Clc1nc(Cl)c2nc[nH]c2n1>>Clc1nc(Cl)c2ncn(C3CCCCO3)c2n1
O1CCCC=C1.ClC1=NC(=C2N=CNC2=N1)Cl.O.C1(=CC=C(C=C1)S(=O)(=O)O)C.C(O)([O-])=O.[Na+]>>ClC1=NC(=C2N=CN(C2=N1)C1OCCCC1)Cl
[CH:10]1=[CH:11][CH2:12][CH2:13][CH2:14][O:15]1.[Cl:1][c:2]1[n:3][c:4]([Cl:5])[c:6]2[n:7][cH:8][nH:9][c:16]2[n:17]1>>[Cl:1][c:2]1[n:3][c:4]([Cl:5])[c:6]2[n:7][cH:8][n:9]([CH:10]3[CH2:11][CH2:12][CH2:13][CH2:14][O:15]3)[c:16]2[n:17]1
C1=COCCC1.Clc1nc(Cl)c2nc[nH]c2n1
Clc1nc(Cl)c2ncn(C3CCCCO3)c2n1
null
null
O.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
833f861fd536c4e2067fdcc1a93d2a1e46416364a06b97cd425c149f7dc60f6d
c37c4c64b8e0c6e5b39694c16f8c97245b55f05530ce8b5df4dfb3a695b50244
c1ncc2ncn(C3CCCCO3)c2n1
[#7;a:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]2:[#7;a:6]:[c:7]:[nH;D2;+0:8]:[c:9]:1:2.[#8:10]1-[C:11]-[C:12]-[C:13]-[CH;D2;+0:14]=[CH;D2;+0:15]-1>>[#7;a:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]2:[#7;a:6]:[c:7]:[n;H0;D3;+0:8](-[CH;D3;+0:15]3-[#8:10]-[C:11]-[C:12]-[C:13]-[CH2;D2;+0:14]-3):[c:9]:1:2
null
[]
50
CELSIUS
null
null
2,6-Dichloro-9H-purine (20 g, 0.11 mol) and 4-toluenesulphonic acid monohydrate (0.2 g) were dissolved in ethyl acetate (300 ml), the mixture heated to 50° C. and a solution of 3,4-dihydro-2H-pyran (12.6 ml, 0.14 mol) in ethyl acetate (50 ml) added slowly over 30 minutes. The reaction mixture was cooled to room tempera...
10.6084/m9.figshare.5104873.v1
null
Ether
Ether
C1=COCCC1.c1ncc2[nH]cnc2n1
c1ncc2[nH]cnc2n1.C1CCOCC1
c1ncc2[nH]cnc2n1.C1CCOCC1
null
O.C(C)(=O)OCC
50
null
C1=COCCC1.Clc1nc(Cl)c2nc[nH]c2n1>O.C(C)(=O)OCC>Clc1nc(Cl)c2ncn(C3CCCCO3)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-403b96eddfb546f98e642649c39d1ee0
Clc1nc(Cl)c2ncn(C3CCCCO3)c2n1.NCC(c1ccccc1)c1ccccc1>>Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
ClC1=NC(=C2N=CN(C2=N1)C1OCCCC1)Cl.C(C)N(C(C)C)C(C)C.C1(=CC=CC=C1)C(CN)C1=CC=CC=C1>>ClC1=NC(=C2N=CN(C2=N1)C1OCCCC1)NCC(C1=CC=CC=C1)C1=CC=CC=C1
Cl[c:4]1[n:3][c:2]([Cl:1])[n:31][c:30]2[c:20]1[n:21][cH:22][n:23]2[CH:24]1[CH2:25][CH2:26][CH2:27][CH2:28][O:29]1.[NH2:5][CH2:6][CH:7]([c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1)[c:14]1[cH:15][cH:16][cH:17][cH:18][cH:19]1>>[Cl:1][c:2]1[n:3][c:4]([NH:5][CH2:6][CH:7]([c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[c:14]2[cH:15...
Clc1nc(Cl)c2ncn(C3CCCCO3)c2n1.NCC(c1ccccc1)c1ccccc1
Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
null
null
C(C)(C)O
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
21d996e324b0e5b6b8600e4cdecb831b9110303de341c2f644de0b809c0bfe6c
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(C(CNc2ncnc3c2ncn3C2CCCCO2)c2ccccc2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5]2:[#7;a:6](-[C:7]-[#8:8]):[c:9]:[#7;a:10]:[c:11]:2:1.[C:12]-[C:13]-[NH2;D1;+0:14]>>[#8:8]-[C:7]-[#7;a:6]1:[c:9]:[#7;a:10]:[c:11]2:[c:5]:1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:2-[NH;D2;+0:14]-[C:13]-[C:12]
104.1
[{"value": 104.1, "product": "ClC1=NC(=C2N=CN(C2=N1)C1OCCCC1)NCC(C1=CC=CC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 2,6-dichloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purine (Preparation 1) (30.9 g, 0.11 mol) in isopropyl alcohol (600 ml) was treated with N-ethyl-N-isopropyl-2-propanamine (47.5 ml, 0.27 mol) and 2,2-diphenylethylamine (24.8 g, 0.13 mol) and the resulting mixture heated under reflux for 3 hours. The solvent w...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ncc2[nH]cnc2n1
c1ncc2[nH]cnc2n1
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOCC1
HCl
C(C)(C)O
null
null
Clc1nc(Cl)c2ncn(C3CCCCO3)c2n1.NCC(c1ccccc1)c1ccccc1>C(C)(C)O>Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-0158caa0433b4a16981a9e69a7155cdb
C[S-].Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>>CSc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
ClC1=NC(=C2N=CN(C2=N1)C1OCCCC1)NCC(C1=CC=CC=C1)C1=CC=CC=C1.C[S-].[Na+]>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)SC)C1OCCCC1)C1=CC=CC=C1
[CH3:1][S-:2].Cl[c:3]1[n:4][c:5]([NH:6][CH2:7][CH:8]([c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[c:21]2[n:22][cH:23][n:24]([CH:25]3[CH2:26][CH2:27][CH2:28][CH2:29][O:30]3)[c:31]2[n:32]1>>[CH3:1][S:2][c:3]1[n:4][c:5]([NH:6][CH2:7][CH:8]([c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14...
C[S-].Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
CSc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
null
null
O.CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
fbee7aea651b2476398ef29f4a72310bd225798f2ee7291e155ba0ec2c32e612
1813ae14fbd9cacead4dcfaf9efbd2467a19b3e216836766b78aa6647dcfb48a
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]-[S-;H0;D1:13]>>[#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](-[S;H0;D2;+0:13]-[C;D1;H3:12]):[#7;a:2]:[c:3]:1:2
99.8
[{"value": 99.8, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)SC)C1OCCCC1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
72
HOUR
A solution of 2-chloro-N-(2,2-diphenylethyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (Preparation 2) (49.7 g, 0.11 mol) in dry N,N-dimethylformamide (200 ml) was treated with sodium thiomethoxide (10 g, 0.14 mol) and the resulting mixture heated under an atmosphere of nitrogen at 100° C. for 90 minutes. The mixtu...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Monosulfide
c1ncc2[nH]cnc2n1
c1ncc2[nH]cnc2n1
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOCC1
Other
O.CN(C=O)C
100
72
C[S-].Clc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>O.CN(C=O)C>CSc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-c6bbeb5096df4e269e3f46d31c8cd773
CSc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>>CS(=O)(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
OOS(=O)[O-].[K+].C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)SC)C1OCCCC1)C1=CC=CC=C1.C(O)([O-])=O.[Na+]>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)S(=O)(=O)C)C1OCCCC1)C1=CC=CC=C1
[CH3:1][S:2][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][n:26]([CH:27]3[CH2:28][CH2:29][CH2:30][CH2:31][O:32]3)[c:33]2[n:34]1>>[CH3:1][S:2](=[O:3])(=[O:4])[c:5]1[n:6][c:7]([NH:8][CH2:9][CH:10]([c:11]2[cH:12][cH:13][cH:...
CSc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
CS(=O)(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
null
null
CC(=O)C.O
Oxidation
OtherReaction
20dd6d48007b4fe7cd760226f21413eb5e71e6468db112596c2e7ea4858c8ac1
5cedc1bf0f43f21d78a249521ecfcec19fc5ac4895c41eed0e84f0c2618149fa
c1ccc(C(CNc2ncnc3c2ncn3C2CCCCO2)c2ccccc2)cc1
[#7;a:1]:[c:2]1:[c:3]:[#7;a:4]:[c:5](-[S;H0;D2;+0:6]-[C;D1;H3:7]):[#7;a:8]:[c:9]:1:[#7;a:10]>>[#7;a:1]:[c:2]1:[c:3]:[#7;a:4]:[c:5](-[S;H0;D4;+0:6](-[C;D1;H3:7])(=[O;D1;H0:11])=[O;D1;H0:12]):[#7;a:8]:[c:9]:1:[#7;a:10]
75.7
[{"value": 75.7, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)S(=O)(=O)C)C1OCCCC1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of Oxone (trade mark) (potassium peroxymonosulphate) (44 g, 71.7 mmol) in water (200 ml) was added dropwise over 2 hours to a solution of N-(2,2-diphenylethyl)-2-(methylsulfanyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (Preparation 3) (25 g, 56.2 mmol) and sodium hydrogencarbonate (20 g, 238 mmol) in a...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfone
null
null
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOCC1
null
CC(=O)C.O
null
null
CSc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>CC(=O)C.O>CS(=O)(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-addae1f9dc0349babc93745e3317e149
CS(=O)(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1.[C-]#N>>N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
O.C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)S(=O)(=O)C)C1OCCCC1)C1=CC=CC=C1.[C-]#N.[K+]>>C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C#N)C1OCCCC1)C1=CC=CC=C1
CS(=O)(=O)[c:3]1[n:4][c:5]([NH:6][CH2:7][CH:8]([c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[c:21]2[n:22][cH:23][n:24]([CH:25]3[CH2:26][CH2:27][CH2:28][CH2:29][O:30]3)[c:31]2[n:32]1.[N:1]#[C-:2]>>[N:1]#[C:2][c:3]1[n:4][c:5]([NH:6][CH2:7][CH:8]([c:9]2[cH:10][cH:11][cH:12][cH:13]...
CS(=O)(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1.[C-]#N
N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
null
null
CN(C=O)C
C-C Coupling
OtherReaction
b7fae133b98238b2705ae50727cb2f9c40d3e25beef0a49c62600e3dc76cb6ce
afc317b75dc27dd96f8b185a6d88494042f714247ebd3d6ce3b0e647608c4473
c1ccc(C(CNc2ncnc3c2ncn3C2CCCCO2)c2ccccc2)cc1
C-S(=O)(=O)-[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-;H0;D1:12]#[N;D1;H0:13]>>[#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;H0;D2;+0:12]#[N;D1;H0:13]):[#7;a:2]:[c:3]:1:2
95.1
[{"value": 95.1, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C#N)C1OCCCC1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
120
CELSIUS
1
HOUR
A solution of N-(2,2-diphenylethyl)-2-(methylsulfonyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (Preparation 4) (20.1 g, 42.1 mmol) in dry N,N-dimethylformamide (100 ml) was treated with potassium cyanide (5.5 g, 84.6 mmol) and the mixture heated at 120° C. for 24 hours under a nitrogen atmosphere. The mixture was...
10.6084/m9.figshare.5104873.v1
null
Sulfone
Nitrile
c1ncc2[nH]cnc2n1
c1ncc2[nH]cnc2n1
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1.C1CCOCC1
HO-
CN(C=O)C
120
1
CS(=O)(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1.[C-]#N>CN(C=O)C>N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-a14d829b1b0f421cb9bd657ac37d643a
N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>>N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
C1(=CC=CC=C1)C(CNC1=C2N=CN(C2=NC(=N1)C#N)C1OCCCC1)C1=CC=CC=C1.Cl>>C1(=CC=CC=C1)C(CNC1=C2N=CNC2=NC(=N1)C#N)C1=CC=CC=C1
C1CCC([n:24]2[cH:23][n:22][c:21]3[c:5]([NH:6][CH2:7][CH:8]([c:9]4[cH:10][cH:11][cH:12][cH:13][cH:14]4)[c:15]4[cH:16][cH:17][cH:18][cH:19][cH:20]4)[n:4][c:3]([C:2]#[N:1])[n:26][c:25]32)OC1>>[N:1]#[C:2][c:3]1[n:4][c:5]([NH:6][CH2:7][CH:8]([c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[c:15]2[cH:16][cH:17][cH:18][cH:19][cH:2...
N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1
N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
null
null
C(C)O
Reduction
OtherReaction
5884540ddb12ce381424fd4d8168e9c573ef97adf4e044c59506f6d05225a030
84394d34c591024a84d9393eb3e8adb8ada5a6225c3abafc4dae9aedd4568be4
c1ccc(C(CNc2ncnc3[nH]cnc23)c2ccccc2)cc1
C1-C-C-C(-[n;H0;D3;+0:1]2:[c:2]:[#7;a:3]:[c:4]3:[c:5]:[#7;a:6]:[c:7]:[#7;a:8]:[c:9]:3:2)-O-C-1>>[#7;a:3]1:[c:2]:[nH;D2;+0:1]:[c:9]2:[#7;a:8]:[c:7]:[#7;a:6]:[c:5]:[c:4]:1:2
99.6
[{"value": 99.6, "product": "C1(=CC=CC=C1)C(CNC1=C2N=CNC2=NC(=N1)C#N)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution of 6-[(2,2-diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2-carbonitrile (Preparation 5) (17 g, 40.1 mmol) in ethanol (850 ml) was treated with 2 N aqueous hydrochloric acid (50 ml) and the mixture stirred at room temperature for 24 hours. The solvent was removed under reduced pressure, the resi...
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
24
N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2ncn(C3CCCCO3)c2n1>C(C)O>N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-6821d444ab2d43739c33dfc175b37f8f
CO.CO.N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1>>COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
C[O-].[Na+].CO.C1(=CC=CC=C1)C(CNC1=C2N=CNC2=NC(=N1)C#N)C1=CC=CC=C1.C[O-].[Na+].CO>>C1(=CC=CC=C1)C(CNC1=C2N=CNC2=NC(=N1)C(=O)OC)C1=CC=CC=C1
[CH3:1][OH:2].C[OH:4].N#[C:3][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][nH:26][c:27]2[n:28]1>>[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][...
CO.CO.N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
null
null
null
Acylation
OtherReaction
632bea7ef0ba9d9c8074dce1accce57a8bc9be8884ed377ae5f21bc270cf078f
94828388e421b34de4961d7ebd23c2a7025dc4ea4c8196535234f20c82fbf8ae
c1ccc(C(CNc2ncnc3[nH]cnc23)c2ccccc2)cc1
C-[OH;D1;+0:1].N#[C;H0;D2;+0:2]-[c:3]1:[#7;a:4]:[c:5](:[#7;a:6]):[c:7](:[#7;a:8]):[c:9]:[#7;a:10]:1.[C;D1;H3:11]-[OH;D1;+0:12]>>[#7;a:8]:[c:7]1:[c:9]:[#7;a:10]:[c:3](-[C;H0;D3;+0:2](=[O;H0;D1;+0:1])-[O;H0;D2;+0:12]-[C;D1;H3:11]):[#7;a:4]:[c:5]:1:[#7;a:6]
null
[]
null
null
24
HOUR
A solution of 6-[(2,2-diphenylethyl)amino]-9H-purine-2-carbonitrile (Preparation 6) (5.0 g, 14.7 mmol) and sodium methoxide (4.0 g, 74.1 mmol) in methanol (300 ml) was heated under reflux for 24 hours. Further sodium methoxide (2.0 g, 37 mmol) and methanol (100 ml) was added and heating continued for a further 24 hours...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Methanol.Methanol
Ester
null
null
c1ccccc1.c1ccccc1.c1ncc2[nH]cnc2n1
Other
null
null
24
CO.CO.N#Cc1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1>>COC(=O)c1nc(NCC(c2ccccc2)c2ccccc2)c2nc[nH]c2n1
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-5ad4245a898440bbbc97f5b29c144228
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](OC(=O)c2ccccc2)[C@H]1OC(=O)c1ccccc1>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O
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)C1=CC=CC=C1)C(=O)OC.C([O-])([O-])=O.[Na+].[Na+]>>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
O=C(c1ccccc1)[O:38][C@H:37]1[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][CH3:34])[n:35][c:36]23)[O:7][C@H:6]([C:4]([NH:3][CH2:2][CH3:1])=[O:5])[C@@H:39]1[O:40]C(=O)c1ccccc1>>[CH3...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](OC(=O)c2ccccc2)[C@H]1OC(=O)c1ccccc1
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O
null
null
CO
Reduction
OtherReaction
0d4a8fd544ba3504cf85ce3b470666ee6956214421e280b154aaf1825d3f9d31
5d3240d328f37074b617f0f9d19c66c4b6d41381ed0bd925b5261a2dcc33ed48
c1ccc(C(CNc2ncnc3c2ncn3[C@H]2CCCO2)c2ccccc2)cc1
O=C(-[O;H0;D2;+0:1]-[C:2]1-[C:3]-[#8:4]-[C:5](-[C:6](-[#7:7])=[O;D1;H0:8])-[C:9]-1-[O;H0;D2;+0:10]-C(=O)-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1>>[#7:7]-[C:6](=[O;D1;H0:8])-[C:5]1-[#8:4]-[C:3]-[C:2](-[OH;D1;+0:1])-[C:9]-1-[OH;D1;+0:10]
98
[{"value": 98.0, "product": "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", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.6, "product": "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", "details": "CALC...
null
null
null
null
A solution of methyl 9-{(2R,3R,4R,5S)-3,4-bis(benzoyloxy)-5-[(ethylamino)carbonyl]-tetrahydro-2-furanyl}-6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 8) (3.4 g, 4.5 mmol) and sodium carbonate (50 mg) in dry methanol (60 ml) was stirred at room temperature for four hours. Solvent was removed under r...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Secondary alcohol.Secondary alcohol
c1ccccc1.c1ccccc1
null
C1CCOC1.c1ccccc1.c1ccccc1.c1ncc2nc[nH]c2n1
HO-
CO
null
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](OC(=O)c2ccccc2)[C@H]1OC(=O)c1ccccc1>CO>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O
ord_dataset-0387783899c642a8b7eb4ba379bcdf5d
ord-69e9be3268244ec6a9f9871f2e034f0a
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NCCN>>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)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(CN)N>>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
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:41]([OH:42])[C@H:39]3[OH:40])[c:38]2[n:37]1)=[O:32].[NH2:33][CH2:34][CH2:35][NH2:36]>>[CH3:1...
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NCCN
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)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]
86.1
[{"value": 86.0, "product": "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", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.1, "product": "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", "details": "CALC...
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) (1.1 g, 2 mmol) and 1,2-ethylenediamine (1.1 g, 18.3 mmol) was heated at 105° C. for 2.5 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
105
null
CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)OC)nc32)[C@H](O)[C@@H]1O.NCCN>ClCCl>CCNC(=O)[C@H]1O[C@@H](n2cnc3c(NCC(c4ccccc4)c4ccccc4)nc(C(=O)NCCN)nc32)[C@H](O)[C@@H]1O