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-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0c41a886f892437a80e1ebfc69bc8999
CCO.CSc1nc(Cl)cc(Cl)n1.Oc1cccc(C(F)(F)F)c1>>CCOc1cc(Oc2cccc(C(F)(F)F)c2)nc(SC)n1
C(C)O.[H-].[Na+].FC(C=1C=C(C=CC1)O)(F)F.[H-].[Na+].ClC1=NC(=NC(=C1)Cl)SC>>C(C)OC1=NC(=NC(=C1)OC1=CC(=CC=C1)C(F)(F)F)SC
[CH3:1][CH2:2][OH:3].Cl[c:4]1[cH:5][c:6](Cl)[n:18][c:19]([S:20][CH3:21])[n:22]1.[OH:7][c:8]1[cH:9][cH:10][cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17]1>>[CH3:1][CH2:2][O:3][c:4]1[cH:5][c:6]([O:7][c:8]2[cH:9][cH:10][cH:11][c:12]([C:13]([F:14])([F:15])[F:16])[cH:17]2)[n:18][c:19]([S:20][CH3:21])[n:22]1
CCO.CSc1nc(Cl)cc(Cl)n1.Oc1cccc(C(F)(F)F)c1
CCOc1cc(Oc2cccc(C(F)(F)F)c2)nc(SC)n1
null
null
CN(C)C=O.C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
29a438eea1e56cb3e58f97b3a65584b92c6780a20719e4a18d7d224393cebeb2
d37fb640deee362662d550188dc8afd00e30441a55a467542ae6bf66e47599da
c1ccc(Oc2ccncn2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[#16:4]):[#7;a:5]:[c;H0;D3;+0:6](-Cl):[c:7]:1.[C;D1;H3:8]-[C:9]-[OH;D1;+0:10].[OH;D1;+0:11]-[c:12](:[c:13]):[c:14]>>[#16:4]-[c:3]1:[#7;a:5]:[c;H0;D3;+0:6](-[O;H0;D2;+0:11]-[c:12](:[c:13]):[c:14]):[c:7]:[c;H0;D3;+0:1](-[O;H0;D2;+0:10]-[C:9]-[C;D1;H3:8]):[#7;a:2]:1
null
[]
null
null
30
MINUTE
Ethanol (1.18 g, 0.0256×1.0 mol) and NaH (1.02 g, (ca.60% in mineral oil), 0.0256×1.0 mol) were dissolved in THF and 4,6-dichloro-2-methylthiopyrimidine (Compound No. VII-23)(5.0 g, 0.0256 mol) was added thereto. The resulting solution was stirred for about 30 minutes at room temperature. To this reaction solution, m-t...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Primary alcohol.Aromatic alcohol
Ether.Ether
c1cncnc1
c1cncnc1
c1cncnc1.c1ccccc1
HCl
CN(C)C=O.C1CCOC1
null
0.5
CCO.CSc1nc(Cl)cc(Cl)n1.Oc1cccc(C(F)(F)F)c1>CN(C)C=O.C1CCOC1>CCOc1cc(Oc2cccc(C(F)(F)F)c2)nc(SC)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-779700042b074f55b42f3a2202e7c555
CSc1nc(Cl)cc(C(F)(F)F)n1.Oc1cccc(C(F)(F)F)c1>>CSc1nc(Oc2cccc(C(F)(F)F)c2)cc(C(F)(F)F)n1
FC(C=1C=C(C=CC1)O)(F)F.[H-].[Na+].ClC1=NC(=NC(=C1)C(F)(F)F)SC>>CSC1=NC(=CC(=N1)C(F)(F)F)OC1=CC(=CC=C1)C(F)(F)F
Cl[c:5]1[n:4][c:3]([S:2][CH3:1])[n:23][c:18]([C:19]([F:20])([F:21])[F:22])[cH:17]1.[OH:6][c:7]1[cH:8][cH:9][cH:10][c:11]([C:12]([F:13])([F:14])[F:15])[cH:16]1>>[CH3:1][S:2][c:3]1[n:4][c:5]([O:6][c:7]2[cH:8][cH:9][cH:10][c:11]([C:12]([F:13])([F:14])[F:15])[cH:16]2)[cH:17][c:18]([C:19]([F:20])([F:21])[F:22])[n:23]1
CSc1nc(Cl)cc(C(F)(F)F)n1.Oc1cccc(C(F)(F)F)c1
CSc1nc(Oc2cccc(C(F)(F)F)c2)cc(C(F)(F)F)n1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
38da1e480b17968341fc50d07104da93d31f20765e3b36e5a0790cb6b1d88a10
27e9a6bab4e3ed54aeb6be4d84cb1c0170208288795e252a46e57e44ecc064f0
c1ccc(Oc2ccncn2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](-[C:6](-[F;D1;H0:7])(-[F;D1;H0:8])-[F;D1;H0:9]):[c:10]:1.[OH;D1;+0:11]-[c:12](:[c:13]):[c:14]>>[F;D1;H0:7]-[C:6](-[F;D1;H0:8])(-[F;D1;H0:9])-[c:5]1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[O;H0;D2;+0:11]-[c:12](:[c:13]):[c:14]):[c:10]:1
null
[]
null
null
null
null
m-(Trifluoromethyl)phenol (1.06 g, 0.0044×1.5 mol) and NaH (0.26 g (ca.60% in mineral oil), 0.0044×1.5 mol) were dissolved in THF, and then 4-chloro-2-methylthio-6-(trifluoromethyl)pyrimidine (Compound No. VII-17) (1.0 g, 0.0044 mol) was added thereto. The resulting solution was refluxed for about 7 hours. The reaction...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic alcohol
Ether
c1cncnc1
c1cncnc1
c1cncnc1.c1ccccc1
HCl
C1CCOC1
null
null
CSc1nc(Cl)cc(C(F)(F)F)n1.Oc1cccc(C(F)(F)F)c1>C1CCOC1>CSc1nc(Oc2cccc(C(F)(F)F)c2)cc(C(F)(F)F)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-3df2c010cc0541928156900e8959ed27
CSc1nc(Br)cc(Br)n1.Oc1cccc(C(F)(F)F)c1>>CSc1nc(Br)cc(Oc2cccc(C(F)(F)F)c2)n1
FC(C=1C=C(C=CC1)O)(F)F.[H-].[Na+].BrC1=NC(=NC(=C1)Br)SC>>BrC1=NC(=NC(=C1)OC1=CC(=CC=C1)C(F)(F)F)SC
Br[c:8]1[cH:7][c:5]([Br:6])[n:4][c:3]([S:2][CH3:1])[n:20]1.[OH:9][c:10]1[cH:11][cH:12][cH:13][c:14]([C:15]([F:16])([F:17])[F:18])[cH:19]1>>[CH3:1][S:2][c:3]1[n:4][c:5]([Br:6])[cH:7][c:8]([O:9][c:10]2[cH:11][cH:12][cH:13][c:14]([C:15]([F:16])([F:17])[F:18])[cH:19]2)[n:20]1
CSc1nc(Br)cc(Br)n1.Oc1cccc(C(F)(F)F)c1
CSc1nc(Br)cc(Oc2cccc(C(F)(F)F)c2)n1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
38da1e480b17968341fc50d07104da93d31f20765e3b36e5a0790cb6b1d88a10
27e9a6bab4e3ed54aeb6be4d84cb1c0170208288795e252a46e57e44ecc064f0
c1ccc(Oc2ccncn2)cc1
Br-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[#16:4]):[#7;a:5]:[c:6](-[Br;D1;H0:7]):[c:8]:1.[OH;D1;+0:9]-[c:10](:[c:11]):[c:12]>>[#16:4]-[c:3]1:[#7;a:2]:[c;H0;D3;+0:1](-[O;H0;D2;+0:9]-[c:10](:[c:11]):[c:12]):[c:8]:[c:6](-[Br;D1;H0:7]):[#7;a:5]:1
null
[]
null
null
null
null
In THF, a phenoxide was prepared from m-(trifluoromethyl)phenol (1.30 g, 0.00794×1.0 mol) and NaH (0.32 g (ca. 60% in mineral oil), 0.00794×1.0 mol), and 4,6-dibromo-2-(methylthio)pyrimidine (Compound No. VII-22) (2.0 g, 0.00794 mol) was added thereto, and the mixture was then allowed to react for 5 hours at room tempe...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic alcohol
Ether
c1cncnc1
c1cncnc1
c1cncnc1.c1ccccc1
HBr
C1CCOC1
null
null
CSc1nc(Br)cc(Br)n1.Oc1cccc(C(F)(F)F)c1>C1CCOC1>CSc1nc(Br)cc(Oc2cccc(C(F)(F)F)c2)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1754134a9e1b4ab5a610540df5e81abc
CC(=O)OC(C)=O.Cc1cccc(N)c1C(=O)O>>CC(=O)Nc1cccc(C)c1C(=O)O
Cl.CC=1C=CC=C(C1C(=O)O)N.[OH-].[Na+].C(C)(=O)OC(C)=O>>CC1=C(C(=O)O)C(=CC=C1)NC(C)=O
CC(=O)O[C:2]([CH3:1])=[O:3].[NH2:4][c:5]1[cH:6][cH:7][cH:8][c:9]([CH3:10])[c:11]1[C:12](=[O:13])[OH:14]>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][cH:8][c:9]([CH3:10])[c:11]1[C:12](=[O:13])[OH:14]
CC(=O)OC(C)=O.Cc1cccc(N)c1C(=O)O
CC(=O)Nc1cccc(C)c1C(=O)O
null
null
O
Acylation
Aminolysis of esters
87d35e51b477fc9a658a6f307eb56d84c8879182772c9dd3a42ec0d584fd2684
627cbc0550c9f51ad0105d9fcf46677e8c93bed87ee95bfe69292a82550c95b7
c1ccccc1
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[c:7]-[C:8](=[O;D1;H0:9])-[O;D1;H1:10]>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[NH;D2;+0:4]-[c:5](:[c:6]):[c:7]-[C:8](=[O;D1;H0:9])-[O;D1;H1:10]
null
[]
null
null
1
HOUR
90.6 g (0.6 mol) of 6-methylanthranilic acid are added to a solution of 24.8 g (0.62 mol) of NaOH in 500 ml of water and 63.4 g (0.62 mol) of acetic anhydride are then added dropwise. After stirring for one hour, the mixture is acidified to pH 3 with conc. HCl with cooling, and the precipitate which deposits is filtere...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Primary amine
Secondary amide
null
null
c1ccccc1
HO-
O
null
1
CC(=O)OC(C)=O.Cc1cccc(N)c1C(=O)O>O>CC(=O)Nc1cccc(C)c1C(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-036dc1bd98f447088e22557193b51876
CC(=O)Nc1cccc(C)c1C(=O)O.O=[N+]([O-])O>>CC(=O)Nc1ccc([N+](=O)[O-])c(C)c1C(=O)O
[N+](=O)(O)[O-].CC1=C(C(=O)O)C(=CC=C1)NC(C)=O>>CC1=C(C(=O)O)C(=CC=C1[N+](=O)[O-])NC(C)=O
[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][cH:8][c:12]([CH3:13])[c:14]1[C:15](=[O:16])[OH:17].O[N+:9](=[O:10])[O-:11]>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][cH:7][c:8]([N+:9](=[O:10])[O-:11])[c:12]([CH3:13])[c:14]1[C:15](=[O:16])[OH:17]
CC(=O)Nc1cccc(C)c1C(=O)O.O=[N+]([O-])O
CC(=O)Nc1ccc([N+](=O)[O-])c(C)c1C(=O)O
null
null
O
Functional Group Addition
Aromatic nitration with HNO3
53848b8b2bb4e867226e49db2e60519b24be9379900e3ad7c56af54fe8fde7a5
ddce49825c02b8965f10c8d99e3c841d26e1f136da6037b417c09313e6d73097
c1ccccc1
O-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3].[C;D1;H3:4]-[c:5](:[c:6]-[C:7](=[O;D1;H0:8])-[O;D1;H1:9]):[cH;D2;+0:10]:[c:11]:[c:12]>>[C;D1;H3:4]-[c:5](:[c:6]-[C:7](=[O;D1;H0:8])-[O;D1;H1:9]):[c;H0;D3;+0:10](-[N+;H0;D3:1](-[O;-;D1;H0:2])=[O;D1;H0:3]):[c:11]:[c:12]
null
[]
10
CELSIUS
1
HOUR
271 ml of 98% nitric acid are initially taken at -5° C. and 106 g (0.55 mol) of the 2-methyl-6-acetamidobenzoic acid prepared in 1. are added in portions. After stirring at 10° C. for one hour, the reaction mixture is poured into a mixture of 540 g of ice and 270 ml of water. The deposited precipitate is filtered off w...
10.6084/m9.figshare.5104873.v1
null
Nitrate
Nitro group
c1ccccc1
c1ccccc1
c1ccccc1
HO-
O
10
1
CC(=O)Nc1cccc(C)c1C(=O)O.O=[N+]([O-])O>O>CC(=O)Nc1ccc([N+](=O)[O-])c(C)c1C(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-36a2a540166a44e2ae3ef4e91516ef3a
CC(=O)Nc1ccc([N+](=O)[O-])c(C)c1C(=O)O>>Cc1c([N+](=O)[O-])ccc(N)c1C(=O)O
CC1=C(C(=O)O)C(=CC=C1[N+](=O)[O-])NC(C)=O.Cl>>CC1=C(C(=O)O)C(=CC=C1[N+](=O)[O-])N
CC(=O)[NH:10][c:9]1[cH:8][cH:7][c:3]([N+:4](=[O:5])[O-:6])[c:2]([CH3:1])[c:11]1[C:12](=[O:13])[OH:14]>>[CH3:1][c:2]1[c:3]([N+:4](=[O:5])[O-:6])[cH:7][cH:8][c:9]([NH2:10])[c:11]1[C:12](=[O:13])[OH:14]
CC(=O)Nc1ccc([N+](=O)[O-])c(C)c1C(=O)O
Cc1c([N+](=O)[O-])ccc(N)c1C(=O)O
null
null
[OH-].[Na+]
Reduction
Hydrogenolysis of amides/imides/carbamates
755df58c254dea764fdda078ffd678ec540bba057c83683be04c253f1270ac7b
025f7cefe51e71668ad5d09fca32df168e9b538347403e4d5c1748073e538adc
c1ccccc1
C-C(=O)-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](=[O;D1;H0:6])-[O;D1;H1:7]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](=[O;D1;H0:6])-[O;D1;H1:7]
null
[]
95
CELSIUS
1
HOUR
450 ml of 2N NaOH are initially taken and 75.6 g (0.317 mol) of 2-methyl-3-nitro-6-acetamidobenzoic acid are added. The reaction mixture is then warmed to 95° C. and is stirred at this temperature for one hour. After cooling to 10° C., it is acidified by addition of 425 ml of 2N HCl, and the precipitate which deposits ...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
Primary amine
null
null
c1ccccc1
HO-
[OH-].[Na+]
95
1
CC(=O)Nc1ccc([N+](=O)[O-])c(C)c1C(=O)O>[OH-].[Na+]>Cc1c([N+](=O)[O-])ccc(N)c1C(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-24a3ddd0c4da4019a874af8b0e5c2e2d
COS(=O)(=O)OC.Cc1c([N+](=O)[O-])ccc(N)c1C(=O)O>>COC(=O)c1c(N)ccc([N+](=O)[O-])c1C
C(=O)=O.S(=O)(=O)(OC)OC.[Na].CC1=C(C(=O)O)C(=CC=C1[N+](=O)[O-])N.C(O)([O-])=O.[Na+].CC1=C(C(=O)O)C(=CC=C1[N+](=O)[O-])N>>CC1=C(C(=O)OC)C(=CC=C1[N+](=O)[O-])N
COS(=O)(=O)O[CH3:1].[OH:2][C:3](=[O:4])[c:5]1[c:6]([NH2:7])[cH:8][cH:9][c:10]([N+:11](=[O:12])[O-:13])[c:14]1[CH3:15]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([NH2:7])[cH:8][cH:9][c:10]([N+:11](=[O:12])[O-:13])[c:14]1[CH3:15]
COS(=O)(=O)OC.Cc1c([N+](=O)[O-])ccc(N)c1C(=O)O
COC(=O)c1c(N)ccc([N+](=O)[O-])c1C
null
null
O.CC(=O)C
Heteroatom Alkylation and Arylation
Methylation of OH with DMS
9474aa79a2adc7353c0c02444ca598a6f486ecdd7ed5edb9ae0645721ee50389
badd4f82161bb0ee7acffd023ea4caae5d036bce7065c10ab0a06e83a6a6f119
c1ccccc1
C-O-S(=O)(=O)-O-[CH3;D1;+0:1].[O;D1;H0:2]=[C:3](-[OH;D1;+0:4])-[c:5]>>[CH3;D1;+0:1]-[O;H0;D2;+0:4]-[C:3](=[O;D1;H0:2])-[c:5]
null
[]
null
null
null
null
49.7 g (0.253 mol) of 2-methyl-3-nitro-6-aminobenzoic acid are dissolved in 380 ml of acetone and 43 g (0.51 mol) of sodium hydrogen carbonate are added. The mixture is then heated to boiling until evolution of CO2 is complete. 35.3 g (0.28 mol) of dimethyl sulfate are then added dropwise in the course of two hours at ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ester
null
null
c1ccccc1
HO-
O.CC(=O)C
null
null
COS(=O)(=O)OC.Cc1c([N+](=O)[O-])ccc(N)c1C(=O)O>O.CC(=O)C>COC(=O)c1c(N)ccc([N+](=O)[O-])c1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9750ebabdd9f4e72aa5a98408ce4247f
COC(=O)c1c(S(=O)(=O)Cl)ccc([N+](=O)[O-])c1C.N>>Cc1c([N+](=O)[O-])ccc2c1C(=O)NS2(=O)=O
N.O.COC(=O)C1=C(C=CC(=C1C)[N+](=O)[O-])S(=O)(=O)Cl>>CC1=C2C(NS(=O)(=O)C2=CC=C1[N+](=O)[O-])=O
CO[C:11]([c:10]1[c:2]([CH3:1])[c:3]([N+:4](=[O:5])[O-:6])[cH:7][cH:8][c:9]1[S:14](Cl)(=[O:15])=[O:16])=[O:12].[NH3:13]>>[CH3:1][c:2]1[c:3]([N+:4](=[O:5])[O-:6])[cH:7][cH:8][c:9]2[c:10]1[C:11](=[O:12])[NH:13][S:14]2(=[O:15])=[O:16]
COC(=O)c1c(S(=O)(=O)Cl)ccc([N+](=O)[O-])c1C.N
Cc1c([N+](=O)[O-])ccc2c1C(=O)NS2(=O)=O
null
null
O1CCCC1
Acylation
OtherReaction
22faaebb6d2314e97dbe234804447317ab111ce22357071da0f15828073371ea
7ccbb14edacd0055aec1ed6cfa3ce7113dc484df701274a79504003cfe511064
O=C1NS(=O)(=O)c2ccccc21
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5](-[S;H0;D4;+0:6](-Cl)(=[O;D1;H0:7])=[O;D1;H0:8]):[c:9].[NH3;D0;+0:10]>>[O;D1;H0:2]=[C;H0;D3;+0:1]1-[NH;D2;+0:10]-[S;H0;D4;+0:6](=[O;D1;H0:7])(=[O;D1;H0:8])-[c:5](:[c:9]):[c:3]-1:[c:4]
null
[]
25
CELSIUS
3
HOUR
104 ml of 25% ammonia solution are initially taken, 100 ml of water are added and a solution of 48.7 g (0.166 mol) of 2-methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride in 70 ml of tetrahydrofuran is then added dropwise at 10° C. After stirring at 25° C. for three hours, the mixture is concentrated on a rotary ...
10.6084/m9.figshare.5104873.v1
null
Ester.Sulfonyl halide
Sulfonamide.Secondary amide
null
c1ccc2c(c1)CNS2
c1ccc2c(c1)CNS2
HCl
O1CCCC1
25
3
COC(=O)c1c(S(=O)(=O)Cl)ccc([N+](=O)[O-])c1C.N>O1CCCC1>Cc1c([N+](=O)[O-])ccc2c1C(=O)NS2(=O)=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-67ec3bcdf85a4cd095b46cc07afa68ed
Cc1c([N+](=O)[O-])ccc2c1C(=O)NS2(=O)=O>>Cc1c(N)ccc2c1C(=O)NS2(=O)=O
CC1=C2C(NS(=O)(=O)C2=CC=C1[N+](=O)[O-])=O.[H][H]>>CC1=C2C(NS(=O)(=O)C2=CC=C1N)=O
O=[N+:4]([O-])[c:3]1[c:2]([CH3:1])[c:8]2[c:7]([cH:6][cH:5]1)[S:12](=[O:13])(=[O:14])[NH:11][C:9]2=[O:10]>>[CH3:1][c:2]1[c:3]([NH2:4])[cH:5][cH:6][c:7]2[c:8]1[C:9](=[O:10])[NH:11][S:12]2(=[O:13])=[O:14]
Cc1c([N+](=O)[O-])ccc2c1C(=O)NS2(=O)=O
Cc1c(N)ccc2c1C(=O)NS2(=O)=O
null
[Pd]
O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C1NS(=O)(=O)c2ccccc21
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
45
CELSIUS
null
null
33.6 g (0.13 mol) of 4-methyl-5-nitrosaccharin are dissolved in 1.2 l of water with warming to 45° C. and 5 g of Pd/C (10% on active carbon) are added. Hydrogen gas is then passed in with vigorous stirring (pressureless hydrogenation). 9 l of H2 are absorbed in the course of 4.5 hours. After cooling to 25° C., the cata...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2c(c1)CNS2
Other
[Pd].O
45
null
Cc1c([N+](=O)[O-])ccc2c1C(=O)NS2(=O)=O>[Pd].O>Cc1c(N)ccc2c1C(=O)NS2(=O)=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-64895c5b03224120a7cbd0bc650559fc
Cc1c(N)ccc2c1C(=O)NS2(=O)=O.[I-]>>Cc1c(I)ccc2c1C(=O)NS2(=O)=O
Cl.[I-].[K+].CC1=C2C(NS(=O)(=O)C2=CC=C1N)=O.N(=O)[O-].[Na+]>>CC1=C2C(NS(=O)(=O)C2=CC=C1I)=O
N[c:3]1[c:2]([CH3:1])[c:8]2[c:7]([cH:6][cH:5]1)[S:12](=[O:13])(=[O:14])[NH:11][C:9]2=[O:10].[I-:4]>>[CH3:1][c:2]1[c:3]([I:4])[cH:5][cH:6][c:7]2[c:8]1[C:9](=[O:10])[NH:11][S:12]2(=[O:13])=[O:14]
Cc1c(N)ccc2c1C(=O)NS2(=O)=O.[I-]
Cc1c(I)ccc2c1C(=O)NS2(=O)=O
null
null
C(C)(=O)O.O
Functional Group Interconversion
OtherReaction
02cafa9f779ee5940bd93b8230c881189907d1a0ec609fabd90735eb4159b16d
9c224743a26d9e1c3135e4817dd611aec414d8ea156f02200a3aef865be78b01
O=C1NS(=O)(=O)c2ccccc21
N-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C;D1;H3:5]):[c:6]-[C:7](=[O;D1;H0:8])-[#7:9].[I-;H0;D0:10]>>[#7:9]-[C:7](=[O;D1;H0:8])-[c:6]:[c:4](-[C;D1;H3:5]):[c;H0;D3;+0:1](-[I;H0;D1;+0:10]):[c:2]:[c:3]
null
[]
50
CELSIUS
null
null
A mixture of 205 ml of glacial acetic acid, 160 ml of water and 40 ml of conc. HCl is initially taken and 23.4 g (0.11 mol) of 4-methyl-5-aminosaccharin are introduced with stirring at 15°-20° C. 7.9 g (0.115 mol) of sodium nitrite are added dropwise to the resulting suspension at 5°-10° C. and it is stirred at 5° C. f...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Aromatic halide
c1ccc2c(c1)CNS2
c1ccc2c(c1)CNS2
c1ccc2c(c1)CNS2
Other
C(C)(=O)O.O
50
null
Cc1c(N)ccc2c1C(=O)NS2(=O)=O.[I-]>C(C)(=O)O.O>Cc1c(I)ccc2c1C(=O)NS2(=O)=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5bfe10bbdded406ba8ad3cc28a98a377
C#CCC(C(=O)OCC)C(=O)c1ccccc1.CNO>>C#CCC1C(=O)N(C)OC1c1ccccc1
[OH-].[Na+].CNO.C(C1=CC=CC=C1)(=O)C(C(=O)OCC)CC#C.[OH-].[Na+].Cl>>CN1OC(C(C1=O)CC#C)C1=CC=CC=C1
CCO[C:5]([CH:4]([CH2:3][C:2]#[CH:1])[C:10](=O)[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)=[O:6].[NH:7]([CH3:8])[OH:9]>>[CH:1]#[C:2][CH2:3][CH:4]1[C:5](=[O:6])[N:7]([CH3:8])[O:9][CH:10]1[c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
C#CCC(C(=O)OCC)C(=O)c1ccccc1.CNO
C#CCC1C(=O)N(C)OC1c1ccccc1
null
null
CCOCC.CO.O
Acylation
OtherReaction
2d3f69240c936c3c2fd9b8f8d3a2721f6df50ac8b98a3bd09cab262d447fc586
56154730fca33738cbd11bdaa7691b6c08e53702809fef7babac3ec4bfd050ad
O=C1CC(c2ccccc2)ON1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4]-[C:5]#[C;D1;H1:6])-[C;H0;D3;+0:7](=O)-[c:8](:[c:9]):[c:10].[C;D1;H3:11]-[NH;D2;+0:12]-[OH;D1;+0:13]>>[C;D1;H1:6]#[C:5]-[C:4]-[C:3]1-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:12](-[C;D1;H3:11])-[O;H0;D2;+0:13]-[CH;D3;+0:7]-1-[c:8](:[c:9]):[c:10]
34.5
[{"value": 34.5, "product": "CN1OC(C(C1=O)CC#C)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-30
CELSIUS
10
MINUTE
A stirred solution of 0.28 g (7.0 mmol) of NaOH in 3 mL of water and 7 mL of methanol was cooled to -30° C. and and a solution of 1.42 g (6.2 mmol) of ethyl α-benzoyl-α-propargylacetate in 2 mL of methanol was added dropwise over 2 min. The mixture was stirred at -30° C. for 10 min and a precooled slurry of 0.54 g (13....
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Secondary amine
Tertiary amide
null
C1C[NH]OC1
C1C[NH]OC1.c1ccccc1
HO-
CCOCC.CO.O
-30
0.166667
C#CCC(C(=O)OCC)C(=O)c1ccccc1.CNO>CCOCC.CO.O>C#CCC1C(=O)N(C)OC1c1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c014829738084401b0a152f2e7cdf4bb
CC(C)(C)NS(=O)(=O)c1cc[nH]c1.CI>>Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
CC(C)(C)NS(=O)(=O)C1=CNC=C1.CI.CC(C)([O-])C.[K+]>>CC(C)(C)NS(=O)(=O)C1=CN(C=C1)C
[nH:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[NH:9][C:10]([CH3:11])([CH3:12])[CH3:13])[cH:14]1.I[CH3:1]>>[CH3:1][n:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[NH:9][C:10]([CH3:11])([CH3:12])[CH3:13])[cH:14]1
CC(C)(C)NS(=O)(=O)c1cc[nH]c1.CI
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
null
null
CN(C=O)C.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
9ead09c93a8a9d57f887a48202e25076c1ec25be9e5b61e0648504d88c26cda6
7a358c636daddc97c1fb4c29f378044d7eac3f01815d9966e599841f642d631a
c1cc[nH]c1
I-[CH3;D1;+0:1].[c:2]1:[c:3]:[c:4]:[c:5]:[nH;D2;+0:6]:1>>[CH3;D1;+0:1]-[n;H0;D3;+0:6]1:[c:2]:[c:3]:[c:4]:[c:5]:1
null
[]
60
CELSIUS
2
HOUR
A solution of N-(1,1-dimethylethyl)-1H-pyrrole-3 -sulfonamide 9 g (0.044 mol) in 90 mL N,N-dimethylforamide was cooled to 15° C. under a nitrogen atmosphere. To this was added 3.2 mL (0.053 mol) of methyl iodide followed by 5.43 g (0.048 mol) of potassium t-butoxide. The mixture was warmed at ca. 60° C. for 2 hours the...
10.6084/m9.figshare.5104873.v1
null
null
null
c1cc[nH]c1
c1cc[nH]c1
c1cc[nH]c1
HI
CN(C=O)C.C(C)(=O)OCC
60
2
CC(C)(C)NS(=O)(=O)c1cc[nH]c1.CI>CN(C=O)C.C(C)(=O)OCC>Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a32d55e896f94ee09bb5a13e0797fb99
COC(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>>COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
CC(C)(C)NS(=O)(=O)C1=CN(C=C1)C.ClC(=O)OC.Cl.C(CCC)[Li]>>CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C(=O)OC
Cl[C:3]([O:2][CH3:1])=[O:4].[cH:5]1[c:6]([S:7](=[O:8])(=[O:9])[NH:10][C:11]([CH3:12])([CH3:13])[CH3:14])[cH:15][cH:16][n:17]1[CH3:18]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([S:7](=[O:8])(=[O:9])[NH:10][C:11]([CH3:12])([CH3:13])[CH3:14])[cH:15][cH:16][n:17]1[CH3:18]
COC(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
null
[Au].[Au]
C1CCOC1
C-C Coupling
Friedel-Crafts acylation
5a20a43a2af69e0af226cfafc54d8480b0d90b850454abf46c572d6de72c336e
25d9bd8621b941df428c033fedc648334f6dc6f4157dff30f33212e6bac7f1de
c1cc[nH]c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4].[#16:5]-[c:6]1:[c:7]:[c:8]:[#7;a:9](-[C;D1;H3:10]):[cH;D2;+0:11]:1>>[#16:5]-[c:6]1:[c:7]:[c:8]:[#7;a:9](-[C;D1;H3:10]):[c;H0;D3;+0:11]:1-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4]
null
[]
-78
CELSIUS
30
MINUTE
To a solution of I g (4.62 mol) of N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 150 mL THF under a nitrogen atmosphere cooled to -78° C. was added dropwise at such a rate as to keep the temperature below -65° C. 4.1 mL (9.48 mmol) 2.32M n-butyllithium in hexanes. The resulting amber turbid solution was st...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether
Ester
c1cc[nH]c1
c1c[nH]cc1
c1c[nH]cc1
HCl
[Au].[Au].C1CCOC1
-78
0.5
COC(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>[Au].[Au].C1CCOC1>COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-476d1b77fb1f4defbab1a8181428d9b8
COC(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>>COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
Cl.CC(C)(C)NS(=O)(=O)C1=CN(C=C1)C.C(CCC)[Li].ClC(=O)OC>>CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C(=O)OC
Cl[C:3]([O:2][CH3:1])=[O:4].[cH:5]1[c:6]([S:7](=[O:8])(=[O:9])[NH:10][C:11]([CH3:12])([CH3:13])[CH3:14])[cH:15][cH:16][n:17]1[CH3:18]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([S:7](=[O:8])(=[O:9])[NH:10][C:11]([CH3:12])([CH3:13])[CH3:14])[cH:15][cH:16][n:17]1[CH3:18]
COC(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
null
[Au].[Au]
C1CCOC1
C-C Coupling
Friedel-Crafts acylation
5a20a43a2af69e0af226cfafc54d8480b0d90b850454abf46c572d6de72c336e
25d9bd8621b941df428c033fedc648334f6dc6f4157dff30f33212e6bac7f1de
c1cc[nH]c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4].[#16:5]-[c:6]1:[c:7]:[c:8]:[#7;a:9](-[C;D1;H3:10]):[cH;D2;+0:11]:1>>[#16:5]-[c:6]1:[c:7]:[c:8]:[#7;a:9](-[C;D1;H3:10]):[c;H0;D3;+0:11]:1-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4]
55.9
[{"value": 55.9, "product": "CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
30
MINUTE
To a solution of 5 g (23 mmol) of N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 150 mL THF under nitrogen atmosphere cooled to -78° C. was added dropwise, at such a rate as to keep the temperature below -65° C., 20 mL (47.4 mmol) 2.32M n-butyllithium in hexanes. The resulting amber turbid solution was stir...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether
Ester
c1cc[nH]c1
c1c[nH]cc1
c1c[nH]cc1
HCl
[Au].[Au].C1CCOC1
-78
0.5
COC(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>[Au].[Au].C1CCOC1>COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-740719404b1e4815a4a77e34574adcd7
COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C>>COC(=O)c1c(S(N)(=O)=O)ccn1C
CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C(=O)OC.FC(C(=O)O)(F)F>>NS(=O)(=O)C1=C(N(C=C1)C)C(=O)OC
CC(C)(C)[NH:8][S:7]([c:6]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[n:13]([CH3:14])[cH:12][cH:11]1)(=[O:9])=[O:10]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[c:6]([S:7]([NH2:8])(=[O:9])=[O:10])[cH:11][cH:12][n:13]1[CH3:14]
COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
COC(=O)c1c(S(N)(=O)=O)ccn1C
null
[Au]
C(Cl)Cl
Deprotection
Tert-butyl deprotection of amine
f7e1da1b4c254f1e6d5afbf8cb56733a4fabd145b80e971e3b7e31007de9e7d6
278d0fb11b582c058ac903379d7fbe11ab8c395937a204965031cf0c344845a9
c1cc[nH]c1
C-C(-C)(-C)-[NH;D2;+0:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c:5]:[c:6]:[#7;a:7]>>[#7;a:7]:[c:6]:[c:5]-[#16:2](-[NH2;D1;+0:1])(=[O;D1;H0:3])=[O;D1;H0:4]
null
[]
null
null
null
null
To a solution of 3.53 g of methyl 3-[[(1,1-dimethylethyl)amino]-sulfonyl]-1-methyl-1H-pyrrole-2-carboxylate in 40 mL, of methylene chloride under an nitrogen atmosphere was added 80 mL of trifluoroacetic acid (TFA). The gold solution was stirred at room temperature overnight ca. 16 hours. The gold solution was concentr...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide
Sulfonamide
null
null
c1c[nH]cc1
Other
[Au].C(Cl)Cl
null
null
COC(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C>[Au].C(Cl)Cl>COC(=O)c1c(S(N)(=O)=O)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ec291f168e3d4ab6bc17d0209ef33361
CSSC.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>>CSc1c(S(=O)(=O)NC(C)(C)C)ccn1C
Cl.C(CCC)[Li].CC(C)(C)NS(=O)(=O)C1=CN(C=C1)C.CSSC>>CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)SC
CS[S:2][CH3:1].[cH:3]1[c:4]([S:5](=[O:6])(=[O:7])[NH:8][C:9]([CH3:10])([CH3:11])[CH3:12])[cH:13][cH:14][n:15]1[CH3:16]>>[CH3:1][S:2][c:3]1[c:4]([S:5](=[O:6])(=[O:7])[NH:8][C:9]([CH3:10])([CH3:11])[CH3:12])[cH:13][cH:14][n:15]1[CH3:16]
CSSC.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
CSc1c(S(=O)(=O)NC(C)(C)C)ccn1C
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
ecf0720e800804680a16cf0e555235641ea38e58156d36aab76023a793ee6569
19099c5abc7af7f1b3d32ffaaaa6b84236f3e8c2bf9cb204008fe61bb9aa47e2
c1cc[nH]c1
C-S-[S;H0;D2;+0:1]-[C;D1;H3:2].[#16:3]-[c:4]1:[c:5]:[c:6]:[#7;a:7](-[C;D1;H3:8]):[cH;D2;+0:9]:1>>[#16:3]-[c:4]1:[c:5]:[c:6]:[#7;a:7](-[C;D1;H3:8]):[c;H0;D3;+0:9]:1-[S;H0;D2;+0:1]-[C;D1;H3:2]
58.8
[{"value": 58.8, "product": "CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)SC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
30
MINUTE
To a solution of 6.48 g (30 mmol) of N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 150 mL THF under nitrogen atmosphere cooled to -78° C. was added dropwise at such a rate as to keep the temperature below -65° C. 25.52 mL (61.5 mmol) 2.41M n-butyllithium in hexanes. The reaction was stirred at -78° C. for ...
10.6084/m9.figshare.5104873.v1
null
Disulfide
Monosulfide
c1cc[nH]c1
c1c[nH]cc1
c1c[nH]cc1
Other
C1CCOC1
-78
0.5
CSSC.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>C1CCOC1>CSc1c(S(=O)(=O)NC(C)(C)C)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ee7d05a9975a483f9332d56b8ce092a7
CSc1c(S(=O)(=O)NC(C)(C)C)ccn1C>>CSc1c(S(N)(=O)=O)ccn1C
CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)SC.FC(C(=O)O)(F)F>>CN1C(=C(C=C1)S(=O)(=O)N)SC
CC(C)(C)[NH:6][S:5]([c:4]1[c:3]([S:2][CH3:1])[n:11]([CH3:12])[cH:10][cH:9]1)(=[O:7])=[O:8]>>[CH3:1][S:2][c:3]1[c:4]([S:5]([NH2:6])(=[O:7])=[O:8])[cH:9][cH:10][n:11]1[CH3:12]
CSc1c(S(=O)(=O)NC(C)(C)C)ccn1C
CSc1c(S(N)(=O)=O)ccn1C
null
null
C(Cl)Cl
Deprotection
Tert-butyl deprotection of amine
f7e1da1b4c254f1e6d5afbf8cb56733a4fabd145b80e971e3b7e31007de9e7d6
278d0fb11b582c058ac903379d7fbe11ab8c395937a204965031cf0c344845a9
c1cc[nH]c1
C-C(-C)(-C)-[NH;D2;+0:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c:5]:[c:6]:[#7;a:7]>>[#7;a:7]:[c:6]:[c:5]-[#16:2](-[NH2;D1;+0:1])(=[O;D1;H0:3])=[O;D1;H0:4]
79.6
[{"value": 79.6, "product": "CN1C(=C(C=C1)S(=O)(=O)N)SC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a solution of 4.63 g (17.66 mmol) N-(1,1-dimethylethyl)-1-methyl-2-(methylthio)-1H-pyrrole-3-sulfonamide in 50 mL of methylene chloride was added 50 mL of trifluoroacetic acid (TFA) under a nitrogen atmosphere. The orange reaction mixture was stirred at room temperature overnight ca. 16 hours. The reaction mixture w...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide
Sulfonamide
null
null
c1c[nH]cc1
Other
C(Cl)Cl
null
16
CSc1c(S(=O)(=O)NC(C)(C)C)ccn1C>C(Cl)Cl>CSc1c(S(N)(=O)=O)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0d425205828e434aa8465064fdc60f2d
BrBr.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>>Cn1ccc(S(=O)(=O)NC(C)(C)C)c1Br
Cl.CC(C)(C)NS(=O)(=O)C1=CN(C=C1)C.C(CCC)[Li].BrBr>>BrC=1N(C=CC1S(=O)(=O)NC(C)(C)C)C
Br[Br:15].[CH3:1][n:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[NH:9][C:10]([CH3:11])([CH3:12])[CH3:13])[cH:14]1>>[CH3:1][n:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[NH:9][C:10]([CH3:11])([CH3:12])[CH3:13])[c:14]1[Br:15]
BrBr.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1Br
null
null
C(C)OCC
Functional Group Interconversion
Bromination
ff11be9c465e8e0b713e91d635a470a31e4b520eecced5f40078ac699b959435
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1cc[nH]c1
Br-[Br;H0;D1;+0:1].[#16:2]-[c:3]1:[c:4]:[c:5]:[#7;a:6](-[C;D1;H3:7]):[cH;D2;+0:8]:1>>[#16:2]-[c:3]1:[c:4]:[c:5]:[#7;a:6](-[C;D1;H3:7]):[c;H0;D3;+0:8]:1-[Br;H0;D1;+0:1]
58.7
[{"value": 58.7, "product": "BrC=1N(C=CC1S(=O)(=O)NC(C)(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
15
MINUTE
To a solution of 8.85 g (41 mmol) of N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 200 mL diethyl ether under a nitrogen atmosphere cooled to -78° C. was added dropwise, at such a rate as to keep the temperature below -65° C., 36.0 mL (85 mmol) 2.41M n-butyllithium in hexanes. The reaction was stirred at -...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1cc[nH]c1
c1c[nH]cc1
c1c[nH]cc1
HBr
C(C)OCC
-78
0.25
BrBr.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>C(C)OCC>Cn1ccc(S(=O)(=O)NC(C)(C)C)c1Br
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-952e75b6acac43568991fc07fe11133a
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1Br>>Cn1ccc(S(N)(=O)=O)c1Br
BrC=1N(C=CC1S(=O)(=O)NC(C)(C)C)C.C(=O)(C(F)(F)F)O>>BrC=1N(C=CC1S(=O)(=O)N)C
CC(C)(C)[NH:7][S:6]([c:5]1[cH:4][cH:3][n:2]([CH3:1])[c:10]1[Br:11])(=[O:8])=[O:9]>>[CH3:1][n:2]1[cH:3][cH:4][c:5]([S:6]([NH2:7])(=[O:8])=[O:9])[c:10]1[Br:11]
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1Br
Cn1ccc(S(N)(=O)=O)c1Br
null
null
C(Cl)Cl
Deprotection
Tert-butyl deprotection of amine
f7e1da1b4c254f1e6d5afbf8cb56733a4fabd145b80e971e3b7e31007de9e7d6
278d0fb11b582c058ac903379d7fbe11ab8c395937a204965031cf0c344845a9
c1cc[nH]c1
C-C(-C)(-C)-[NH;D2;+0:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c:5]:[c:6]:[#7;a:7]>>[#7;a:7]:[c:6]:[c:5]-[#16:2](-[NH2;D1;+0:1])(=[O;D1;H0:3])=[O;D1;H0:4]
21.4
[{"value": 21.4, "product": "BrC=1N(C=CC1S(=O)(=O)N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a solution of 7.11 g (24 mmol) of 2-bromo-N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 50 mL methylene chloride under a nitrogen atmosphere was added 50 mL of TFA. The reaction mixture was allowed to stir at room temperature overnight ca. 16 hours. The reaction mixture was concentrated in vacuo. Three ...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide
Sulfonamide
null
null
c1c[nH]cc1
Other
C(Cl)Cl
null
16
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1Br>C(Cl)Cl>Cn1ccc(S(N)(=O)=O)c1Br
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1689ec83ac2b4e2e9bc10359a96a617b
CN(C)C=O.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>>Cn1ccc(S(=O)(=O)NC(C)(C)C)c1C=O
CC(C)(C)NS(=O)(=O)C1=CN(C=C1)C.CN(C=O)C.Cl>>CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C=O
CN(C)[CH:15]=[O:16].[CH3:1][n:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[NH:9][C:10]([CH3:11])([CH3:12])[CH3:13])[cH:14]1>>[CH3:1][n:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[NH:9][C:10]([CH3:11])([CH3:12])[CH3:13])[c:14]1[CH:15]=[O:16]
CN(C)C=O.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1C=O
null
null
C1CCOC1
C-C Coupling
OtherReaction
d9d66c0383111c39672c6f97615b03ec6c6d4177c1f7428c4be4b53020a617e2
f0bd75a0630092c31f21f61f4a015c77ae0dff14a0b742b4370d7a38fda490f7
c1cc[nH]c1
C-N(-C)-[CH;D2;+0:1]=[O;D1;H0:2].[#16:3]-[c:4]1:[c:5]:[c:6]:[#7;a:7](-[C;D1;H3:8]):[cH;D2;+0:9]:1>>[#16:3]-[c:4]1:[c:5]:[c:6]:[#7;a:7](-[C;D1;H3:8]):[c;H0;D3;+0:9]:1-[CH;D2;+0:1]=[O;D1;H0:2]
39
[{"value": 39.0, "product": "CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
30
MINUTE
To a solution of 12.96 g (60 mmol) of N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 300 mL THF under a nitrogen atmosphere cooled to -78° C. was added dropwise, at such a rate as to keep the temperature below -65° C., 52.35 mL (123 mmol) 2.35M n-butylithium in hexanes. The reaction was stirred at -78° C. f...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
Aldehyde
c1cc[nH]c1
c1c[nH]cc1
c1c[nH]cc1
Other
C1CCOC1
-78
0.5
CN(C)C=O.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>C1CCOC1>Cn1ccc(S(=O)(=O)NC(C)(C)C)c1C=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-3b75f1f1033143b794c5a9db7bc6a994
CON.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1C=O>>CON=Cc1[nH]ccc1S(=O)(=O)NC(C)(C)C
O.C(C)(=O)[O-].[Na+].Cl.CON.CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C=O>>CC(C)(C)NS(=O)(=O)C1=C(NC=C1)C=NOC
[CH3:1][O:2][NH2:3].C[n:6]1[c:5]([CH:4]=O)[c:9]([S:10](=[O:11])(=[O:12])[NH:13][C:14]([CH3:15])([CH3:16])[CH3:17])[cH:8][cH:7]1>>[CH3:1][O:2][N:3]=[CH:4][c:5]1[nH:6][cH:7][cH:8][c:9]1[S:10](=[O:11])(=[O:12])[NH:13][C:14]([CH3:15])([CH3:16])[CH3:17]
CON.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1C=O
CON=Cc1[nH]ccc1S(=O)(=O)NC(C)(C)C
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
6615c49504af75b4b6922f41afffb4a5b99652fa7cae8476b66064dff8f82dfd
3d6c7b6a0f29252ce5dcda36fa3ef05efc366c421f47850a88ae430c686fc79d
c1cc[nH]c1
C-[n;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[c:5]:1-[CH;D2;+0:6]=O.[C;D1;H3:7]-[#8:8]-[NH2;D1;+0:9]>>[C;D1;H3:7]-[#8:8]-[N;H0;D2;+0:9]=[CH;D2;+0:6]-[c:5]1:[c:4]:[c:3]:[c:2]:[nH;D2;+0:1]:1
96.2
[{"value": 96.2, "product": "CC(C)(C)NS(=O)(=O)C1=C(NC=C1)C=NOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a suspension of 3.91 g (46.8 mmol) of methoxyamine hydrochloride in 60 mL of methanol was added 3.84 g (46.8 mmol) of sodium acetate. After stirring the white suspension for ca. 15 minutes 5.72 g (23 mmol) of N-(1,1-dimethylethyl)-2-formyl-1-methyl-1H-pyrrole-3-sulfonamide was added in one portion. The white suspens...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine
null
c1c[nH]cc1
c1cc[nH]c1
c1cc[nH]c1
HO-
CO
null
null
CON.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1C=O>CO>CON=Cc1[nH]ccc1S(=O)(=O)NC(C)(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0d13730de7524a88a677102766469c81
CON=Cc1[nH]ccc1S(=O)(=O)NC(C)(C)C>>CON=Cc1c(S(N)(=O)=O)ccn1C
CC(C)(C)NS(=O)(=O)C1=C(NC=C1)C=NOC.C(=O)(C(F)(F)F)O>>CON=CC=1N(C=CC1S(=O)(=O)N)C
C[C:14](C)(C)[NH:8][S:7]([c:6]1[c:5]([CH:4]=[N:3][O:2][CH3:1])[nH:13][cH:12][cH:11]1)(=[O:9])=[O:10]>>[CH3:1][O:2][N:3]=[CH:4][c:5]1[c:6]([S:7]([NH2:8])(=[O:9])=[O:10])[cH:11][cH:12][n:13]1[CH3:14]
CON=Cc1[nH]ccc1S(=O)(=O)NC(C)(C)C
CON=Cc1c(S(N)(=O)=O)ccn1C
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
20cc103add3cd1e006adea631b88681acfdc5c9577152885a8f7e1af33d45e2d
28816b3b9482e4d163df59e58124d148a1ad8c4cd722815a1176060bd8f7cbeb
c1cc[nH]c1
C-[C;H0;D4;+0:1](-C)(-C)-[NH;D2;+0:2]-[#16:3](=[O;D1;H0:4])(=[O;D1;H0:5])-[c:6]1:[c:7]:[c:8]:[nH;D2;+0:9]:[c:10]:1-[C:11]=[#7:12]>>[#7:12]=[C:11]-[c:10]1:[c:6](-[#16:3](-[NH2;D1;+0:2])(=[O;D1;H0:4])=[O;D1;H0:5]):[c:7]:[c:8]:[n;H0;D3;+0:9]:1-[CH3;D1;+0:1]
null
[]
null
null
16
HOUR
To a solution of 5.74 g (21.9 mmol) of N-(1,1-dimethylethyl)-2-[(methoxyimino)-methyl]-1H-pyrrole-3-sulfonamide in 75 mL methylene chloride under a nitrogen atmosphere was add 75 mL of TFA. The clear orange reaction mixture was allowed to stir at room temperature overnight ca. 16 hours. The orange reaction mixture was ...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide
Sulfonamide
c1cc[nH]c1
c1c[nH]cc1
c1c[nH]cc1
Other
C(Cl)Cl
null
16
CON=Cc1[nH]ccc1S(=O)(=O)NC(C)(C)C>C(Cl)Cl>CON=Cc1c(S(N)(=O)=O)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-00887c12283747658f3f8ff3622cc7d7
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1.O=S=O>>CN(C)S(=O)(=O)c1c(S(N)(=O)=O)c(C(C)(C)C)cn1C
ClN1C(CCC1=O)=O.C(CCC)[Li].CC(C)(C)NS(=O)(=O)C1=CN(C=C1)C.O1CCCC1.S(=O)=O>>CC(C)(C)C=1C(=C(N(C1)C)S(=O)(=O)N(C)C)S(=O)(=O)N
[cH:7]1[c:8]([S:9]([NH:10][C:14]([CH3:15])([CH3:16])[CH3:17])(=[O:11])=[O:12])[cH:13][cH:18][n:19]1[CH3:20].[S:4](=[O:5])=[O:6]>>[CH3:1][N:2]([CH3:3])[S:4](=[O:5])(=[O:6])[c:7]1[c:8]([S:9]([NH2:10])(=[O:11])=[O:12])[c:13]([C:14]([CH3:15])([CH3:16])[CH3:17])[cH:18][n:19]1[CH3:20]
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1.O=S=O
CN(C)S(=O)(=O)c1c(S(N)(=O)=O)c(C(C)(C)C)cn1C
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
dd02c072c1999fa8686995b4042f04e221b8deebf71bf2d4552560d128d10b13
93bbbd43c2c285e6277a373ccd60ddc62a63bc9ef6f7404d9d43a73dd3e65412
c1cc[nH]c1
[C;D1;H3:1]-[C;H0;D4;+0:2](-[C;D1;H3:3])(-[C;D1;H3:4])-[NH;D2;+0:5]-[#16:6](=[O;D1;H0:7])(=[O;D1;H0:8])-[c:9]1:[cH;D2;+0:10]:[c:11]:[#7;a:12](-[C;D1;H3:13]):[cH;D2;+0:14]:1.[O;D1;H0:15]=[S;H0;D2;+0:16]=[O;D1;H0:17]>>[C;D1;H3:1]-[C;H0;D4;+0:2](-[C;D1;H3:3])(-[C;D1;H3:4])-[c;H0;D3;+0:10]1:[c:11]:[#7;a:12](-[C;D1;H3:13]):...
null
[]
null
null
1
HOUR
A solution of 6.48 g (30 mmol) of N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 150 mL of anhydrous tetrahydrofuran (THF) under nitrogen atmosphere was cooled to -78° C. The colorless reaction was treated with 61.5 mmol of 2.38M n-butyllithium in hexanes dropwise at such a rate as to keep the temperature b...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide
Sulfonamide.Tertiary amine
c1cc[nH]c1
c1cc[nH]c1
c1cc[nH]c1
null
null
null
1
Cn1ccc(S(=O)(=O)NC(C)(C)C)c1.O=S=O>>CN(C)S(=O)(=O)c1c(S(N)(=O)=O)c(C(C)(C)C)cn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-bce13e6e0f2b4556bf712059577ecdcd
CN(C)S(=O)(=O)c1c(S(N)(=O)=O)c(C(C)(C)C)cn1C>>CN(C)S(=O)(=O)c1c(S(N)(=O)=O)ccn1C
CC(C)(C)C=1C(=C(N(C1)C)S(=O)(=O)N(C)C)S(=O)(=O)N.C(=O)(C(F)(F)F)O>>CN(S(=O)(=O)C=1N(C=CC1S(=O)(=O)N)C)C
CC(C)(C)[c:13]1[c:8]([S:9]([NH2:10])(=[O:11])=[O:12])[c:7]([S:4]([N:2]([CH3:1])[CH3:3])(=[O:5])=[O:6])[n:15]([CH3:16])[cH:14]1>>[CH3:1][N:2]([CH3:3])[S:4](=[O:5])(=[O:6])[c:7]1[c:8]([S:9]([NH2:10])(=[O:11])=[O:12])[cH:13][cH:14][n:15]1[CH3:16]
CN(C)S(=O)(=O)c1c(S(N)(=O)=O)c(C(C)(C)C)cn1C
CN(C)S(=O)(=O)c1c(S(N)(=O)=O)ccn1C
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
f537e285e05ca146260582b82dd7145f92fed17d878e360c64814f979252e9c0
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1cc[nH]c1
C-C(-C)(-C)-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3](-[C;D1;H3:4]):[c:5](-[#16:6]):[c:7]:1-[#16:8]>>[#16:6]-[c:5]1:[#7;a:3](-[C;D1;H3:4]):[c:2]:[cH;D2;+0:1]:[c:7]:1-[#16:8]
null
[]
null
null
16
HOUR
To a solution of 6.95 g (21 mmol) of N3 -(1,1-dimethylethyl)-N2,N2,1-trimethyl-1H-pyrrole-2,3-disulfonamide in 75 mL of methylene chloride under a nitrogen atmosphere was added 75 mL of TFA. The reaction mixture was allowed to stir at room temperature overnight ca. 16 hours. The reaction mixture was concentrated in vac...
10.6084/m9.figshare.5104873.v1
null
null
null
c1cc[nH]c1
c1c[nH]cc1
c1c[nH]cc1
Other
C(Cl)Cl
null
16
CN(C)S(=O)(=O)c1c(S(N)(=O)=O)c(C(C)(C)C)cn1C>C(Cl)Cl>CN(C)S(=O)(=O)c1c(S(N)(=O)=O)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-acf44331951a4df6acd00502ec327265
CN(C)C(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>>CN(C)C(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
[Cl-].[NH4+].C(CCC)[Li].CC(C)(C)NS(=O)(=O)C1=CN(C=C1)C.CN(C(=O)Cl)C.Cl>>CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C(=O)N(C)C
Cl[C:4]([N:2]([CH3:1])[CH3:3])=[O:5].[cH:6]1[c:7]([S:8](=[O:9])(=[O:10])[NH:11][C:12]([CH3:13])([CH3:14])[CH3:15])[cH:16][cH:17][n:18]1[CH3:19]>>[CH3:1][N:2]([CH3:3])[C:4](=[O:5])[c:6]1[c:7]([S:8](=[O:9])(=[O:10])[NH:11][C:12]([CH3:13])([CH3:14])[CH3:15])[cH:16][cH:17][n:18]1[CH3:19]
CN(C)C(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1
CN(C)C(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
null
null
C1CCOC1
C-C Coupling
Friedel-Crafts acylation
c62ead7f39f71b7724860484b46753891098edf9d1881789884a9b80b0963d93
5aa1746bf699ea29bafc1c026df78788a454dbf70414dd42e98cfe9c89871a23
c1cc[nH]c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C;D1;H3:4])-[C;D1;H3:5].[#16:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10](-[C;D1;H3:11]):[cH;D2;+0:12]:1>>[#16:6]-[c:7]1:[c:8]:[c:9]:[#7;a:10](-[C;D1;H3:11]):[c;H0;D3;+0:12]:1-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#7:3](-[C;D1;H3:4])-[C;D1;H3:5]
50.2
[{"value": 50.2, "product": "CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C(=O)N(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
30
MINUTE
To a solution of 6.48 g (30 mmol) of N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-3-sulfonamide in 150 mL THF under a nitrogen atmosphere cooled to -78° C. was added dropwise, at such a rate as to keep the temperature below -60° C., 25 mL (61.5 mmol) 2.46M n-butyllithium in hexanes. The reaction mixture was stirred at -78...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Tertiary amide
Tertiary amide
c1cc[nH]c1
c1c[nH]cc1
c1c[nH]cc1
HCl
C1CCOC1
-78
0.5
CN(C)C(=O)Cl.Cn1ccc(S(=O)(=O)NC(C)(C)C)c1>C1CCOC1>CN(C)C(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4d0fbf7c4db24ef2820d2d87a9754e6c
CN(C)C(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C>>CN(C)C(=O)c1c(S(N)(=O)=O)ccn1C
CC(C)(C)NS(=O)(=O)C1=C(N(C=C1)C)C(=O)N(C)C.C(=O)(C(F)(F)F)O>>NS(=O)(=O)C1=C(N(C=C1)C)C(=O)N(C)C
CC(C)(C)[NH:9][S:8]([c:7]1[c:6]([C:4]([N:2]([CH3:1])[CH3:3])=[O:5])[n:14]([CH3:15])[cH:13][cH:12]1)(=[O:10])=[O:11]>>[CH3:1][N:2]([CH3:3])[C:4](=[O:5])[c:6]1[c:7]([S:8]([NH2:9])(=[O:10])=[O:11])[cH:12][cH:13][n:14]1[CH3:15]
CN(C)C(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C
CN(C)C(=O)c1c(S(N)(=O)=O)ccn1C
null
null
C(Cl)Cl
Deprotection
Tert-butyl deprotection of amine
f7e1da1b4c254f1e6d5afbf8cb56733a4fabd145b80e971e3b7e31007de9e7d6
278d0fb11b582c058ac903379d7fbe11ab8c395937a204965031cf0c344845a9
c1cc[nH]c1
C-C(-C)(-C)-[NH;D2;+0:1]-[#16:2](=[O;D1;H0:3])(=[O;D1;H0:4])-[c:5]:[c:6]:[#7;a:7]>>[#7;a:7]:[c:6]:[c:5]-[#16:2](-[NH2;D1;+0:1])(=[O;D1;H0:3])=[O;D1;H0:4]
92.9
[{"value": 92.9, "product": "NS(=O)(=O)C1=C(N(C=C1)C)C(=O)N(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a solution of 5.63 g of 3-[[(1,1-dimethylethyl)amino]sulfonyl]-N,N,1-trimethyl-1H-pyrrole-2-carboxamide in 75 mL of methylene chloride was added 75 mL of TFA. The reaction mixture was allowed to stir at room temperature overnight ca. 16 hours. The reaction mixture was concentrated in vacuo. Three portions of diethyl...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide
Sulfonamide
null
null
c1c[nH]cc1
Other
C(Cl)Cl
null
16
CN(C)C(=O)c1c(S(=O)(=O)NC(C)(C)C)ccn1C>C(Cl)Cl>CN(C)C(=O)c1c(S(N)(=O)=O)ccn1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-66c80b7eb0654eda89cb0773db258c7f
CC(C)(C)N.Cn1cccc1.O=S=O>>Cn1cccc1S(=O)(=O)NC(C)(C)C
S(=O)=O.C(CCC)[Li].CN1C=CC=C1.C(C)(C)(C)N>>CC(C)(C)NS(=O)(=O)C=1N(C=CC1)C
[NH2:10][C:11]([CH3:12])([CH3:13])[CH3:14].[CH3:1][n:2]1[cH:3][cH:4][cH:5][cH:6]1.[S:7](=[O:8])=[O:9]>>[CH3:1][n:2]1[cH:3][cH:4][cH:5][c:6]1[S:7](=[O:8])(=[O:9])[NH:10][C:11]([CH3:12])([CH3:13])[CH3:14]
CC(C)(C)N.Cn1cccc1.O=S=O
Cn1cccc1S(=O)(=O)NC(C)(C)C
null
null
C1CCOC1
Protection
OtherReaction
7e3b061ab6a31649fa6a371fc4433b0fe652714813be2bfca8beb3fa97e8bfe0
95f9bec41996e1d6385bdfda8a285b8770de8952829289a8e8fac2bb61b0a5ce
c1cc[nH]c1
[C;D1;H3:1]-[#7;a:2]1:[c:3]:[c:4]:[c:5]:[cH;D2;+0:6]:1.[C;D1;H3:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[NH2;D1;+0:11].[O;D1;H0:12]=[S;H0;D2;+0:13]=[O;D1;H0:14]>>[C;D1;H3:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[NH;D2;+0:11]-[S;H0;D4;+0:13](=[O;D1;H0:12])(=[O;D1;H0:14])-[c;H0;D3;+0:6]1:[c:5]:[c:4]:[c:3]:[#7;a:2]:1-[C;D1;H3...
28.5
[{"value": 28.5, "product": "CC(C)(C)NS(=O)(=O)C=1N(C=CC1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
A solution of 10 g (0.12 mol) of N-methyl-pyrrole in 120 mL of anhydrous THF under nitrogen atmosphere was cooled to below -70° C. then treated with 56 mL of 2.4M n-butyllithium in hexanes (0.13 mol) dropwise at such a rate as to keep the temperature below -60° C. The resulting brown colored mixture was stirred for 16 ...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Sulfonamide
c1cc[nH]c1
c1ccc[nH]1
c1ccc[nH]1
null
C1CCOC1
null
16
CC(C)(C)N.Cn1cccc1.O=S=O>C1CCOC1>Cn1cccc1S(=O)(=O)NC(C)(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-eaa9d1d720194b459594019c4118fe86
COC(=O)Cl.Cn1cccc1S(=O)(=O)NC(C)(C)C>>COC(=O)c1ccn(C)c1S(=O)(=O)NC(C)(C)C
ClC(=O)OC.CC(C)(C)NS(=O)(=O)C=1N(C=CC1)C.C(CCC)[Li]>>CC(C)(C)NS(=O)(=O)C=1N(C=CC1C(=O)OC)C
Cl[C:3]([O:2][CH3:1])=[O:4].[cH:5]1[cH:6][cH:7][n:8]([CH3:9])[c:10]1[S:11](=[O:12])(=[O:13])[NH:14][C:15]([CH3:16])([CH3:17])[CH3:18]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][n:8]([CH3:9])[c:10]1[S:11](=[O:12])(=[O:13])[NH:14][C:15]([CH3:16])([CH3:17])[CH3:18]
COC(=O)Cl.Cn1cccc1S(=O)(=O)NC(C)(C)C
COC(=O)c1ccn(C)c1S(=O)(=O)NC(C)(C)C
null
null
C1CCOC1.C(C)(=O)OCC
C-C Coupling
Friedel-Crafts acylation
50a128be0ecdfa440a20704024d0efb90098e7c5cc7f1747307f8056462cd7b3
25d9bd8621b941df428c033fedc648334f6dc6f4157dff30f33212e6bac7f1de
c1cc[nH]c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4].[#16:5]-[c:6]1:[cH;D2;+0:7]:[c:8]:[c:9]:[#7;a:10]:1-[C;D1;H3:11]>>[#16:5]-[c:6]1:[#7;a:10](-[C;D1;H3:11]):[c:9]:[c:8]:[c;H0;D3;+0:7]:1-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C;D1;H3:4]
14.3
[{"value": 14.3, "product": "CC(C)(C)NS(=O)(=O)C=1N(C=CC1C(=O)OC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 2.5 g (11.5 mmol) of N-(1,1-dimethylethyl)-1-methyl-1H-pyrrole-2-sulfonamide in 50 mL THF under nitrogen atmosphere cooled to below -70° C. was added dropwise 13 mL (32.5 mmol) of 2.5M n-butyllithium at such a rate as to keep the temperature below -58° C. After stirring at -20° C. to -10° C. for 30 min...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether
Ester
c1ccc[nH]1
c1c[nH]cc1
c1c[nH]cc1
HCl
C1CCOC1.C(C)(=O)OCC
null
0.5
COC(=O)Cl.Cn1cccc1S(=O)(=O)NC(C)(C)C>C1CCOC1.C(C)(=O)OCC>COC(=O)c1ccn(C)c1S(=O)(=O)NC(C)(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a5a19d2e3ccc4cb7bff13f06f043ffc0
COC(=O)c1ccn(C)c1S(N)(=O)=O.COc1nc(C)nc(NC(=O)Oc2ccccc2)n1>>COC(=O)c1ccn(C)c1S(=O)(=O)NC(=O)NC1=NC(OC)=CN(C)N1
Cl.NS(=O)(=O)C=1N(C=CC1C(=O)OC)C.COC1=NC(=NC(=N1)C)NC(OC1=CC=CC=C1)=O.C1CCC2=NCCCN2CC1>>COC=1N=C(NN(C1)C)NC(=O)NS(=O)(=O)C=1N(C=CC1C(=O)OC)C
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][n:8]([CH3:9])[c:10]1[S:11](=[O:12])(=[O:13])[NH2:14].c1ccc(O[C:15](=[O:16])[NH:17][c:18]2[n:19][c:20]([O:21][CH3:22])[n:24][c:23]([CH3:25])[n:26]2)cc1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][n:8]([CH3:9])[c:10]1[S:11](=[O:12])(=[O:13])[NH:14][C:15](=[O:16])[NH:17][C:18]1...
COC(=O)c1ccn(C)c1S(N)(=O)=O.COc1nc(C)nc(NC(=O)Oc2ccccc2)n1
COC(=O)c1ccn(C)c1S(=O)(=O)NC(=O)NC1=NC(OC)=CN(C)N1
null
null
C(C)#N.O
Acylation
OtherReaction
f988767444e9fb806a783801e95d85a36d79f56e5189ed5c36171ed46c73d7c8
d4aa065d3dd6b2eb9aa239fb936ebd84810693bbeac61ec007c62593188be20b
O=C(NC1=NC=CNN1)NS(=O)(=O)c1ccc[nH]1
[#7;a:1]:[c:2]-[#16:3](-[NH2;D1;+0:4])(=[O;D1;H0:5])=[O;D1;H0:6].[C;D1;H3:7]-[#8:8]-[c;H0;D3;+0:9]1:[n;H0;D2;+0:10]:[c;H0;D3;+0:11](-[#7:12]-[C;H0;D3;+0:13](=[O;D1;H0:14])-O-c2:c:c:c:c:c:2):[n;H0;D2;+0:15]:[c;H0;D3;+0:16](-[CH3;D1;+0:17]):[n;H0;D2;+0:18]:1>>[#7;a:1]:[c:2]-[#16:3](=[O;D1;H0:5])(=[O;D1;H0:6])-[NH;D2;+0:4...
null
[]
null
null
30
MINUTE
Methyl 2-(aminosulfonyl)-1-methyl-1H-pyrrole-3-carboxylate (0.10 g, 0.46 mmol) and 0.13 g (0.50 mmol) of phenyl (4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate were combined in 2 mL of acetonitrile and 0.075 mL of DBU was added and the resulting amber solution was stirred at ambient temperature for 30 min. The reactio...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Carbamic ester.Ether.Ether
Enamine.Sulfonamide.Hydrazine.Ether.Urea
c1ccccc1.c1ncncn1
C1=C[NH]NC=N1
c1c[nH]cc1.C1=C[NH]NC=N1
HO-
C(C)#N.O
null
0.5
COC(=O)c1ccn(C)c1S(N)(=O)=O.COc1nc(C)nc(NC(=O)Oc2ccccc2)n1>C(C)#N.O>COC(=O)c1ccn(C)c1S(=O)(=O)NC(=O)NC1=NC(OC)=CN(C)N1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-819df65591774363bb9b76f5effae47b
CC(=O)c1c(F)cccc1F.Nc1ncccc1C=O>>Fc1cccc(F)c1-c1ccc2cccnc2n1
NC1=C(C=O)C=CC=N1.CC(=O)C1=C(C=CC=C1F)F.[OH-].[K+]>>FC1=C(C(=CC=C1)F)C1=NC2=NC=CC=C2C=C1
O=[C:9]([c:8]1[c:2]([F:1])[cH:3][cH:4][cH:5][c:6]1[F:7])[CH3:10].O=[CH:11][c:12]1[cH:13][cH:14][cH:15][n:16][c:17]1[NH2:18]>>[F:1][c:2]1[cH:3][cH:4][cH:5][c:6]([F:7])[c:8]1-[c:9]1[cH:10][cH:11][c:12]2[cH:13][cH:14][cH:15][n:16][c:17]2[n:18]1
CC(=O)c1c(F)cccc1F.Nc1ncccc1C=O
Fc1cccc(F)c1-c1ccc2cccnc2n1
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
3936808456ac378e4397a3dafa777312a8f9677e9b37312d1a52d94356865178
08667cf58f28cec17f3f2604bf85c92e5fab0f09949cef6990e380a70b99d0bf
c1ccc(-c2ccc3cccnc3n2)cc1
O=[C;H0;D3;+0:1](-[CH3;D1;+0:2])-[c;H0;D3;+0:3](:[c:4](-[F;D1;H0:5]):[c:6]):[c:7](-[F;D1;H0:8]):[c:9].O=[CH;D2;+0:10]-[c:11](:[c:12]):[c:13](-[NH2;D1;+0:14]):[#7;a:15]:[c:16]>>[F;D1;H0:5]-[c:4](:[c:6]):[c;H0;D3;+0:3](-[c;H0;D3;+0:1]1:[cH;D2;+0:2]:[cH;D2;+0:10]:[c:11](:[c:12]):[c:13](:[#7;a:15]:[c:16]):[n;H0;D2;+0:14]:1...
79
[{"value": 79.0, "product": "FC1=C(C(=CC=C1)F)C1=NC2=NC=CC=C2C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.4, "product": "FC1=C(C(=CC=C1)F)C1=NC2=NC=CC=C2C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Aminonicotinaldehyde (2.44 g, 20 mmol) and 2,6-difluoroacetophenone (3.28 g, 21 mmol) are dissolved in 20 ml of MeOH. The mixture is treated dropwise with 3 ml of 40% KOH and, after the exothermic reaction has subsided, it is poured onto water and the residue which is deposited is filtered off with suction. 3.8 g (79...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone.Primary amine
null
c1ccncc1
c1cnc2ncccc2c1
c1ccccc1.c1cnc2ncccc2c1
HO-
CO
null
null
CC(=O)c1c(F)cccc1F.Nc1ncccc1C=O>CO>Fc1cccc(F)c1-c1ccc2cccnc2n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6da8fccbc46d48d9b47085df7224e0c2
CC(=O)c1nccs1.Nc1ncccc1C=O>>c1cnc2nc(-c3nccs3)ccc2c1
NC1=C(C=O)C=CC=N1.C(C)(=O)C=1SC=CN1.[OH-].[K+]>>S1C(=NC=C1)C1=NC2=NC=CC=C2C=C1
O=[C:6]([c:7]1[n:8][cH:9][cH:10][s:11]1)[CH3:12].O=[CH:13][c:14]1[c:4]([NH2:5])[n:3][cH:2][cH:1][cH:15]1>>[cH:1]1[cH:2][n:3][c:4]2[n:5][c:6](-[c:7]3[n:8][cH:9][cH:10][s:11]3)[cH:12][cH:13][c:14]2[cH:15]1
CC(=O)c1nccs1.Nc1ncccc1C=O
c1cnc2nc(-c3nccs3)ccc2c1
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
3936808456ac378e4397a3dafa777312a8f9677e9b37312d1a52d94356865178
08667cf58f28cec17f3f2604bf85c92e5fab0f09949cef6990e380a70b99d0bf
c1cnc2nc(-c3nccs3)ccc2c1
O=[C;H0;D3;+0:1](-[CH3;D1;+0:2])-[c;H0;D3;+0:3]1:[#16;a:4]:[c:5]:[c:6]:[#7;a:7]:1.O=[CH;D2;+0:8]-[c:9](:[c:10]):[c:11](-[NH2;D1;+0:12]):[#7;a:13]:[c:14]>>[c:10]:[c:9]1:[cH;D2;+0:8]:[cH;D2;+0:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:3]2:[#16;a:4]:[c:5]:[c:6]:[#7;a:7]:2):[n;H0;D2;+0:12]:[c:11]:1:[#7;a:13]:[c:14]
46.5
[{"value": 46.0, "product": "S1C(=NC=C1)C1=NC2=NC=CC=C2C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 46.5, "product": "S1C(=NC=C1)C1=NC2=NC=CC=C2C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
2-Aminonicotinaldehyde (1.5 g, 12.3 mmol) and 2-acetylthiazole (1.64 g, 12.9 mmol) are dissolved in 12 ml of MeOH and the mixture is treated with 1.5 ml of 40% KOH. After 3 h, the reaction is complete and the mixture is poured onto water. The solid which is deposited is filtered off with suction, washed and dried. 1.22...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone.Primary amine
null
c1ccncc1
c1cnc2ncccc2c1
c1cnc2ncccc2c1.c1cscn1
HO-
CO
null
3
CC(=O)c1nccs1.Nc1ncccc1C=O>CO>c1cnc2nc(-c3nccs3)ccc2c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4fe7e7b0295444c08046dd75241f89c9
C[C@]12CC(=NO)C(=O)C[C@@H]1CC[C@@H]1[C@@H]2CC[C@]2(C)[C@@H](O)CC[C@@H]12.NO>>CC(=O)O[C@H]1CC[C@H]2[C@@H]3CC[C@H]4CC(=NO)C(=NO)C[C@]4(C)[C@H]3CC[C@]12C
ON=C1C(C[C@@H]2CC[C@H]3[C@@H]4CC[C@@H]([C@@]4(C)CC[C@@H]3[C@]2(C1)C)O)=O.NO.Cl.CC(=O)[O-].[Na+].O>>C(C)(=O)O[C@@H]1[C@]2(C)[C@@H](CC1)[C@@H]1CC[C@H]3CC(C(C[C@]3(C)[C@H]1CC2)=NO)=NO
O=[C:14]1[CH2:13][C@@H:12]2[CH2:11][CH2:10][C@H:9]3[C@@H:8]4[CH2:7][CH2:6][C@H:5]([OH:4])[C@@:26]4([CH3:27])[CH2:25][CH2:24][C@@H:23]3[C@@:21]2([CH3:22])[CH2:20][C:17]1=[N:18][OH:19].[NH2:15][OH:16]>>[CH3:1][C:2](=[O:3])[O:4][C@H:5]1[CH2:6][CH2:7][C@H:8]2[C@@H:9]3[CH2:10][CH2:11][C@H:12]4[CH2:13][C:14](=[N:15][OH:16])[...
C[C@]12CC(=NO)C(=O)C[C@@H]1CC[C@@H]1[C@@H]2CC[C@]2(C)[C@@H](O)CC[C@@H]12.NO
CC(=O)O[C@H]1CC[C@H]2[C@@H]3CC[C@H]4CC(=NO)C(=NO)C[C@]4(C)[C@H]3CC[C@]12C
null
null
O
Acylation
OtherReaction
b4a23b040d618e2b4c65b8ca220b611623f5b0d1aab9edd43720ddfd6dc65183
11bb0537b70e084630323c94e955c7bfcb0b78dbd257b5953e091be00486ff45
N=C1CC2[C@@H](CC[C@H]3[C@@H]4CCCC4CC[C@H]23)CC1=N
O=[C;H0;D3;+0:1](-[C:2]-[C:3])-[C:4](=[#7:5]-[O;D1;H1:6])-[C:7].[C:8]-[C:9](-[OH;D1;+0:10])-[C:11].[NH2;D1;+0:12]-[O;D1;H1:13]>>[C:8]-[C:9](-[O;H0;D2;+0:10]-[C:14](-[C;D1;H3:15])=[O;D1;H0:16])-[C:11].[C:3]-[C:2]-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[O;D1;H1:13])-[C:4](=[#7:5]-[O;D1;H1:6])-[C:7]
null
[]
null
null
null
null
A suspension of steroid 7, NH2OH.HCl and NaOAc/H2O was refluxed for 20 minutes. The reaction was cooled to room temperature and poured into H2O. The precipitate was collected by filtration. The resulting solid 8 was washed with H2O and air and dried; wt. 23.4 g. Conditions: See reaction.notes.procedure_details. Workup:...
10.6084/m9.figshare.5104873.v1
null
Ketone.Secondary alcohol.Primary amine
Ester.Oxime
C1CC[C@H]2[C@H](C1)CC[C@@H]1[C@@H]2CC[C@@H]2CCC[C@H]21
C1CC[C@H]2[C@H](C1)CC[C@@H]1[C@@H]2CC[C@@H]2CCC[C@H]21
C1CC[C@H]2[C@H](C1)CC[C@@H]1[C@@H]2CC[C@@H]2CCC[C@H]21
null
O
null
null
C[C@]12CC(=NO)C(=O)C[C@@H]1CC[C@@H]1[C@@H]2CC[C@]2(C)[C@@H](O)CC[C@@H]12.NO>O>CC(=O)O[C@H]1CC[C@H]2[C@@H]3CC[C@H]4CC(=NO)C(=NO)C[C@]4(C)[C@H]3CC[C@]12C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9c0049ffd5bd4c2597bd8dc1da4f9125
N#Cc1c([N+](=O)[O-])cccc1[N+](=O)[O-].Sc1ccccc1>>N#Cc1c(Sc2ccccc2)cccc1[N+](=O)[O-]
[N+](=O)([O-])C1=C(C#N)C(=CC=C1)[N+](=O)[O-].C1(=CC=CC=C1)S.C(=O)([O-])[O-].[K+].[K+].N1=CC=CC=C1>>[N+](=O)([O-])C1=C(C#N)C(=CC=C1)SC1=CC=CC=C1
O=[N+]([O-])[c:4]1[c:3]([C:2]#[N:1])[c:15]([N+:16](=[O:17])[O-:18])[cH:14][cH:13][cH:12]1.[SH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1>>[N:1]#[C:2][c:3]1[c:4]([S:5][c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[cH:12][cH:13][cH:14][c:15]1[N+:16](=[O:17])[O-:18]
N#Cc1c([N+](=O)[O-])cccc1[N+](=O)[O-].Sc1ccccc1
N#Cc1c(Sc2ccccc2)cccc1[N+](=O)[O-]
null
null
CN(C)C=O.O
Heteroatom Alkylation and Arylation
OtherReaction
a4feeb0224c95b591ffae5f38900a0e1c2efd3e17e75ff223366faab4cc7a260
124c5e2fa17ef87ad2270619dfa07e40ca83ae69e72cfb81a511ef39c15c3695
c1ccc(Sc2ccccc2)cc1
O=[N+](-[O-])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[SH;D1;+0:8]-[c:9](:[c:10]):[c:11]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[S;H0;D2;+0:8]-[c:9](:[c:10]):[c:11]):[c:2]:[c:3]
89
[{"value": 89.0, "product": "[N+](=O)([O-])C1=C(C#N)C(=CC=C1)SC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.7, "product": "[N+](=O)([O-])C1=C(C#N)C(=CC=C1)SC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
An ice water bath-cooled mixture of 2.0 g (0.01 mol) of 2,6-dinitrobenzonitrile (Lancaster Synthesis, Inc., Windham, N.H. 03087), 1.06 ml (0.01 mol) of thiophenol, and 1.44 g (0.01 mol) of anhydrous K2CO3 in 50 mL of DMF was stirred for 0.5 h. Pyridine was added to the reaction mixture until it became basic, and was fo...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Aromatic thiol
Monosulfide
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HO-
CN(C)C=O.O
null
0.5
N#Cc1c([N+](=O)[O-])cccc1[N+](=O)[O-].Sc1ccccc1>CN(C)C=O.O>N#Cc1c(Sc2ccccc2)cccc1[N+](=O)[O-]
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d850da0197e245649bff3ba3999f661f
N#Cc1c(Sc2ccccc2)cccc1[N+](=O)[O-]>>N#Cc1c(N)cccc1Sc1ccccc1
O.[N+](=O)([O-])C1=C(C#N)C(=CC=C1)SC1=CC=CC=C1.Cl[Sn]Cl>>NC1=C(C#N)C(=CC=C1)SC1=CC=CC=C1
O=[N+:5]([O-])[c:4]1[c:3]([C:2]#[N:1])[c:9]([S:10][c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[cH:8][cH:7][cH:6]1>>[N:1]#[C:2][c:3]1[c:4]([NH2:5])[cH:6][cH:7][cH:8][c:9]1[S:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
N#Cc1c(Sc2ccccc2)cccc1[N+](=O)[O-]
N#Cc1c(N)cccc1Sc1ccccc1
null
null
COCCOCCOC.Cl
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(Sc2ccccc2)cc1
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
To a water bath-cooled solution of 3.9 g (0.015 mol) of 2-nitro-6-(phenylthio)benzonitrile (Example 1) in 85 mL of diglyme was added dropwise, with stirring, 11.53 g (0.045 mol) of SnCl2.2H2 O in 35 mL of conc. HCl. The water bath was removed, and the reaction was stirred at room temperature for 0.5 h. This reaction mi...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccccc1
Other
COCCOCCOC.Cl
null
null
N#Cc1c(Sc2ccccc2)cccc1[N+](=O)[O-]>COCCOCCOC.Cl>N#Cc1c(N)cccc1Sc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-942c876021324f25bb9887685a674993
Cc1cc(C)cc(S)c1.N#Cc1c([N+](=O)[O-])cccc1[N+](=O)[O-]>>Cc1cc(C)cc(Sc2cccc([N+](=O)[O-])c2C#N)c1
O.[N+](=O)([O-])C1=C(C#N)C(=CC=C1)[N+](=O)[O-].C(=O)([O-])[O-].[K+].[K+].CC=1C=C(C=C(C1)C)S>>CC=1C=C(C=C(C1)C)SC1=C(C#N)C(=CC=C1)[N+](=O)[O-]
[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([SH:8])[cH:20]1.O=[N+]([O-])[c:9]1[cH:10][cH:11][cH:12][c:13]([N+:14](=[O:15])[O-:16])[c:17]1[C:18]#[N:19]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([S:8][c:9]2[cH:10][cH:11][cH:12][c:13]([N+:14](=[O:15])[O-:16])[c:17]2[C:18]#[N:19])[cH:20]1
Cc1cc(C)cc(S)c1.N#Cc1c([N+](=O)[O-])cccc1[N+](=O)[O-]
Cc1cc(C)cc(Sc2cccc([N+](=O)[O-])c2C#N)c1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
a4feeb0224c95b591ffae5f38900a0e1c2efd3e17e75ff223366faab4cc7a260
124c5e2fa17ef87ad2270619dfa07e40ca83ae69e72cfb81a511ef39c15c3695
c1ccc(Sc2ccccc2)cc1
O=[N+](-[O-])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[SH;D1;+0:8]-[c:9](:[c:10]):[c:11]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[S;H0;D2;+0:8]-[c:9](:[c:10]):[c:11]):[c:2]:[c:3]
73,011.2
[{"value": 80.0, "product": "CC=1C=C(C=C(C1)C)SC1=C(C#N)C(=CC=C1)[N+](=O)[O-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73011.2, "product": "CC=1C=C(C=C(C1)C)SC1=C(C#N)C(=CC=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
A mixture of 2,6-dinitrobenzonitrile (1.4 g 7.2 mmol) and K2CO3 (1.1 g, 7.9 mmol) in 10 ml of DMF was chilled to 0° C. A solution of 3,5-dimethylthiophenol (1.1 g 0.0079 mmol) in 10 ml of DMF, was added dropwise over 30 min with stirring under nitrogen. After stirring an additional 30 min, the reaction mixture was pour...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Aromatic thiol
Monosulfide
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HO-
CN(C)C=O
0
null
Cc1cc(C)cc(S)c1.N#Cc1c([N+](=O)[O-])cccc1[N+](=O)[O-]>CN(C)C=O>Cc1cc(C)cc(Sc2cccc([N+](=O)[O-])c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8c04216a28bb4609b9208e0d1a14c091
Cc1cc(C)cc(Sc2cccc([N+](=O)[O-])c2C#N)c1>>Cc1cc(C)cc(Sc2cccc(N)c2C#N)c1
CC=1C=C(C=C(C1)C)SC1=C(C#N)C(=CC=C1)[N+](=O)[O-].[OH-].[Na+]>>NC1=C(C#N)C(=CC=C1)SC1=CC(=CC(=C1)C)C
O=[N+:14]([O-])[c:13]1[cH:12][cH:11][cH:10][c:9]([S:8][c:7]2[cH:6][c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:18]2)[c:15]1[C:16]#[N:17]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([S:8][c:9]2[cH:10][cH:11][cH:12][c:13]([NH2:14])[c:15]2[C:16]#[N:17])[cH:18]1
Cc1cc(C)cc(Sc2cccc([N+](=O)[O-])c2C#N)c1
Cc1cc(C)cc(Sc2cccc(N)c2C#N)c1
null
null
COCCOCCOC.O.Cl
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(Sc2ccccc2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
64
[{"value": 64.0, "product": "NC1=C(C#N)C(=CC=C1)SC1=CC(=CC(=C1)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 64.0, "product": "NC1=C(C#N)C(=CC=C1)SC1=CC(=CC(=C1)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-[(3,5-Dimethylphenyl)thio]-6-nitrobenzonitrile (Example 5) (1.0 g, 0.0035 mol) was dissolved in 50 ml of diglyme. A solution of stannous chloride-2H2O (3.16 g, 0.014 mol) in 15 ml of concentrated HCl was added dropwise with stirring. After stirring 1 h and 15 min, the reaction mixture was poured into a solution of 12...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccccc1
Other
COCCOCCOC.O.Cl
null
null
Cc1cc(C)cc(Sc2cccc([N+](=O)[O-])c2C#N)c1>COCCOCCOC.O.Cl>Cc1cc(C)cc(Sc2cccc(N)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a610715a9a2049339b2b5008fb407eed
COc1cccc(Sc2cccc(F)c2C#N)c1.O=C(OO)c1cccc(Cl)c1.O=C(OO)c1cccc(Cl)c1>>COc1cccc(S(=O)(=O)c2cccc(F)c2C#N)c1
ClC1=CC(=CC=C1)C(=O)OO.S([O-])(O)=O.[Na+].O.FC1=C(C#N)C(=CC=C1)SC1=CC(=CC=C1)OC.ClC1=CC(=CC=C1)C(=O)OO>>FC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC=C1)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([S:8][c:11]2[cH:12][cH:13][cH:14][c:15]([F:16])[c:17]2[C:18]#[N:19])[cH:20]1.O=C(O[OH:10])c1cccc(Cl)c1.OOC(c1cccc(Cl)c1)=[O:9]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][cH:14][c:15]([F:16])[c:17]2[C:18]#[N:19])[cH:20]1
COc1cccc(Sc2cccc(F)c2C#N)c1.O=C(OO)c1cccc(Cl)c1.O=C(OO)c1cccc(Cl)c1
COc1cccc(S(=O)(=O)c2cccc(F)c2C#N)c1
null
null
null
Oxidation
OtherReaction
fa9379080be52796ca8aad2066720360879b6743ff6ce008e4ef793c8196487b
00d01750cba21c0937a6facb86295b3305f6895167f97bd162720af7670b1a25
O=S(=O)(c1ccccc1)c1ccccc1
Cl-c1:c:c:c:c(-C(=O)-O-[OH;D1;+0:1]):c:1.Cl-c1:c:c:c:c(-C(=[O;H0;D1;+0:2])-O-O):c:1.[c:3]:[c:4](-[S;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]):[c:9]>>[O;H0;D1;+0:1]=[S;H0;D4;+0:5](=[O;H0;D1;+0:2])(-[c:4](:[c:3]):[c:9])-[c:6](:[c:7]):[c:8]
null
[]
null
null
null
null
To a solution of 2 g (7.7 mmol) of 2-fluoro-6-[(3-methoxyphenyl)thio]benzonitrile (Example 13) was added 2.93 g (17 mmol) of m-chloroperbenzoic acid. The resultant mixture was stirred for 24 h. Additional 0.29 g of m-chloroperbenzoic acid was added and the resultant mixture was stirred for 15 min. Excess sodium bisulfi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Peroxide.Peroxide.Monosulfide
Sulfone
c1ccccc1.c1ccccc1
null
c1ccccc1.c1ccccc1
HCl
null
null
null
COc1cccc(Sc2cccc(F)c2C#N)c1.O=C(OO)c1cccc(Cl)c1.O=C(OO)c1cccc(Cl)c1>>COc1cccc(S(=O)(=O)c2cccc(F)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-70d2fe8819214856a573963ea6b87bb1
COc1cccc(S(=O)(=O)c2cccc(F)c2C#N)c1.[NH4+]>>COc1cccc(S(=O)(=O)c2cccc(N)c2C#N)c1
FC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC=C1)OC.[NH4+].[OH-]>>NC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC=C1)OC
F[c:15]1[cH:14][cH:13][cH:12][c:11]([S:8]([c:7]2[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[cH:20]2)(=[O:9])=[O:10])[c:17]1[C:18]#[N:19].[NH4+:16]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][cH:14][c:15]([NH2:16])[c:17]2[C:18]#[N:19])[cH:20]1
COc1cccc(S(=O)(=O)c2cccc(F)c2C#N)c1.[NH4+]
COc1cccc(S(=O)(=O)c2cccc(N)c2C#N)c1
null
null
CO.CCO
Functional Group Interconversion
OtherReaction
0b3f36c6e96a844ac8c671a85ab317446ee29bfa735a32d39184f4616cac3a55
560c85d40afb1a57d77cf3258abf3be5bba829f35224f8687bf9a1d4c1f94bd9
O=S(=O)(c1ccccc1)c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[NH4+;D0:8]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[NH2;D1;+0:8]):[c:2]:[c:3]
null
[]
130
CELSIUS
null
null
To a solution of 0.7 g (2.4 mmol) of 2-fluoro-6-[(3-methoxyphenyl)sulfonyl]benzonitrile (Example 14) in 110 ml of MeOH/EtOH (7:4) was added 20 mL of concentrated NH4OH, This mixture was sealed in a glass-lined bomb and heated at 130° C. for 3 h. After solvent removal, the resultant concentrate was purified by flash col...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HF
CO.CCO
130
null
COc1cccc(S(=O)(=O)c2cccc(F)c2C#N)c1.[NH4+]>CO.CCO>COc1cccc(S(=O)(=O)c2cccc(N)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f52f628e55bf48349560d5f7350120df
COc1cccc(Sc2cccc(F)c2C#N)c1>>COc1cccc(S(=O)c2cccc(F)c2C#N)c1
ClC1=CC(=CC=C1)C(=O)OO.S([O-])(O)=O.[Na+].FC1=C(C#N)C(=CC=C1)SC1=CC(=CC=C1)OC.ClC1=CC(=CC=C1)C(=O)OO>>FC1=C(C#N)C(=CC=C1)S(=O)C1=CC(=CC=C1)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([S:8][c:10]2[cH:11][cH:12][cH:13][c:14]([F:15])[c:16]2[C:17]#[N:18])[cH:19]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([S:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([F:15])[c:16]2[C:17]#[N:18])[cH:19]1
COc1cccc(Sc2cccc(F)c2C#N)c1
COc1cccc(S(=O)c2cccc(F)c2C#N)c1
null
null
O
Oxidation
Sulfanyl to sulfinyl
9edfaf6d72a81452ea8e3a1cdcb10a58409fff36608e97019e7273998b3d5373
f5f6bb6ca76a2267cd589767b4d67e7a17ab1ac383eeb6143dcd5d92e00e1b6a
O=S(c1ccccc1)c1ccccc1
[c:1]:[c:2](-[S;H0;D2;+0:3]-[c:4](:[c:5]):[c:6]):[c:7]>>[O;D1;H0:8]=[S;H0;D3;+0:3](-[c:2](:[c:1]):[c:7])-[c:4](:[c:5]):[c:6]
null
[]
null
null
null
null
To a solution of 2 g (7.7 mmol) of 2-fluoro-6-[(3-methoxyphenyl)thio]benzonitrile (Example 13) was added portionwise 1.6 g (9.3 mmol) of m-chloroperbenzoic acid. The resultant mixture was stirred for 24 h. Additional 0.16 g of m-chloroperbenzoic acid was added and the resultant mixture was stirred for 15 min. Excess so...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfoxide
null
null
c1ccccc1.c1ccccc1
null
O
null
null
COc1cccc(Sc2cccc(F)c2C#N)c1>O>COc1cccc(S(=O)c2cccc(F)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-efbec65196ea4c25a91fe4f5f0f30b06
COc1cccc(S(=O)c2cccc(F)c2C#N)c1.[NH4+]>>COc1cccc(S(=O)c2cccc(N)c2C#N)c1
FC1=C(C#N)C(=CC=C1)S(=O)C1=CC(=CC=C1)OC.[NH4+].[OH-]>>NC1=C(C#N)C(=CC=C1)S(=O)C1=CC(=CC=C1)OC
F[c:14]1[cH:13][cH:12][cH:11][c:10]([S:8]([c:7]2[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[cH:19]2)=[O:9])[c:16]1[C:17]#[N:18].[NH4+:15]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([S:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([NH2:15])[c:16]2[C:17]#[N:18])[cH:19]1
COc1cccc(S(=O)c2cccc(F)c2C#N)c1.[NH4+]
COc1cccc(S(=O)c2cccc(N)c2C#N)c1
null
null
CO.CCO
Functional Group Interconversion
OtherReaction
0b3f36c6e96a844ac8c671a85ab317446ee29bfa735a32d39184f4616cac3a55
560c85d40afb1a57d77cf3258abf3be5bba829f35224f8687bf9a1d4c1f94bd9
O=S(c1ccccc1)c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[NH4+;D0:8]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[NH2;D1;+0:8]):[c:2]:[c:3]
null
[]
130
CELSIUS
null
null
To a solution of 0.73 g (2.7 mmol) of 2-fluoro-6-[(3-methoxyphenyl)sulfinyl]benzonitrile (Example 16) in 65 ml of MeOH/EtOH (2.5:4) was added 20 mL of concentrated NH4OH. This mixture was sealed in a glass-lined bomb and heated at 130° C. for 3 h. After solvent removal, the resultant concentrate was purified by flash c...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HF
CO.CCO
130
null
COc1cccc(S(=O)c2cccc(F)c2C#N)c1.[NH4+]>CO.CCO>COc1cccc(S(=O)c2cccc(N)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6ddfb59c25f34fe781aa3d4f78fc3efa
Cc1cc(C)cc(Sc2cccc(F)c2C#N)c1>>Cc1cc(C)cc(S(=O)c2cccc(F)c2C#N)c1
CC=1C=C(C=C(C1)C)SC1=C(C#N)C(=CC=C1)F.OOS(=O)[O-].[K+]>>CC=1C=C(C=C(C1)C)S(=O)C1=C(C#N)C(=CC=C1)F
[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([S:8][c:10]2[cH:11][cH:12][cH:13][c:14]([F:15])[c:16]2[C:17]#[N:18])[cH:19]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([S:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([F:15])[c:16]2[C:17]#[N:18])[cH:19]1
Cc1cc(C)cc(Sc2cccc(F)c2C#N)c1
Cc1cc(C)cc(S(=O)c2cccc(F)c2C#N)c1
null
null
CO.O
Oxidation
Sulfanyl to sulfinyl
9edfaf6d72a81452ea8e3a1cdcb10a58409fff36608e97019e7273998b3d5373
f5f6bb6ca76a2267cd589767b4d67e7a17ab1ac383eeb6143dcd5d92e00e1b6a
O=S(c1ccccc1)c1ccccc1
[c:1]:[c:2](-[S;H0;D2;+0:3]-[c:4](:[c:5]):[c:6]):[c:7]>>[O;D1;H0:8]=[S;H0;D3;+0:3](-[c:2](:[c:1]):[c:7])-[c:4](:[c:5]):[c:6]
47
[{"value": 47.0, "product": "CC=1C=C(C=C(C1)C)S(=O)C1=C(C#N)C(=CC=C1)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile (Example 18) (1.0 g, 3.9 mmol) was dissolved in 100 ml of methanol. A solution of OXONE®.dagger. (2.63 g, 4.3 mmol) in 15 ml of water was added dropwise with stirring. After stirring 1.5 h, the solid was removed by vacuum filtration and washed with 3×50 ml of methanol. ...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfoxide
null
null
c1ccccc1.c1ccccc1
null
CO.O
null
null
Cc1cc(C)cc(Sc2cccc(F)c2C#N)c1>CO.O>Cc1cc(C)cc(S(=O)c2cccc(F)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-3a63765ce57f4be88697886cd8f75569
Cc1cc(C)cc(Sc2cccc(F)c2C#N)c1>>Cc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1
O.OOS(=O)[O-].[K+].CC=1C=C(C=C(C1)C)SC1=C(C#N)C(=CC=C1)F.OOS(=O)[O-].[K+]>>CC=1C=C(C=C(C1)C)S(=O)(=O)C1=C(C#N)C(=CC=C1)F
[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([S:8][c:11]2[cH:12][cH:13][cH:14][c:15]([F:16])[c:17]2[C:18]#[N:19])[cH:20]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][cH:14][c:15]([F:16])[c:17]2[C:18]#[N:19])[cH:20]1
Cc1cc(C)cc(Sc2cccc(F)c2C#N)c1
Cc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1
null
null
CO
Oxidation
OtherReaction
20dd6d48007b4fe7cd760226f21413eb5e71e6468db112596c2e7ea4858c8ac1
5cedc1bf0f43f21d78a249521ecfcec19fc5ac4895c41eed0e84f0c2618149fa
O=S(=O)(c1ccccc1)c1ccccc1
[c:1]:[c:2](-[S;H0;D2;+0:3]-[c:4](:[c:5]):[c:6]):[c:7]>>[O;D1;H0:8]=[S;H0;D4;+0:3](=[O;D1;H0:9])(-[c:2](:[c:1]):[c:7])-[c:4](:[c:5]):[c:6]
65
[{"value": 65.0, "product": "CC=1C=C(C=C(C1)C)S(=O)(=O)C1=C(C#N)C(=CC=C1)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile (Example 18) (1.0 g 3.9 mmol) was dissolved in 100 ml of methanol. A solution of OXONE®.dagger. (5.26 g, 8.6 mmol) in 30 ml of water was added dropwise with stirring. After stirring 1 h, another 1.5 equivalents of OXONE® (3.60 g 5.9 mmol) was added. The reaction was sti...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfone
null
null
c1ccccc1.c1ccccc1
null
CO
null
null
Cc1cc(C)cc(Sc2cccc(F)c2C#N)c1>CO>Cc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ba9711ed922e47f3840d3a080575bd49
Cc1cc(C)cc(S(=O)c2cccc(F)c2C#N)c1.N>>Cc1cc(C)cc(S(=O)c2cccc(N)c2C#N)c1
CCOC(=O)C.CC=1C=C(C=C(C1)C)S(=O)C1=C(C#N)C(=CC=C1)F.N>>NC1=C(C#N)C(=CC=C1)S(=O)C1=CC(=CC(=C1)C)C
F[c:14]1[cH:13][cH:12][cH:11][c:10]([S:8]([c:7]2[cH:6][c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:19]2)=[O:9])[c:16]1[C:17]#[N:18].[NH3:15]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([S:8](=[O:9])[c:10]2[cH:11][cH:12][cH:13][c:14]([NH2:15])[c:16]2[C:17]#[N:18])[cH:19]1
Cc1cc(C)cc(S(=O)c2cccc(F)c2C#N)c1.N
Cc1cc(C)cc(S(=O)c2cccc(N)c2C#N)c1
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
5cea7b75c7f95cc50fd74029efa1cddce51f01200160afa4aaecfa45e52a1621
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
O=S(c1ccccc1)c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[NH3;D0;+0:8]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[NH2;D1;+0:8]):[c:2]:[c:3]
61
[{"value": 61.0, "product": "NC1=C(C#N)C(=CC=C1)S(=O)C1=CC(=CC(=C1)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 59.2, "product": "NC1=C(C#N)C(=CC=C1)S(=O)C1=CC(=CC(=C1)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
null
null
2-[(3,5-Dimethylphenyl)sulfinyl]-6-fluorobenzonitrile (Example 19) (0.4 g, 1.5 mmol) was dissolved in 40 ml of methanol and chilled to -78° C. Condensed ammonia (20 ml, 15.4 g, 905 mmol) was added and the mixture was heated to 150° C. in a sealed Parr bomb for 24 h. Chromatography on silica gel (flash; Hex/EtOAc 1:1) p...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HF
CO
-78
null
Cc1cc(C)cc(S(=O)c2cccc(F)c2C#N)c1.N>CO>Cc1cc(C)cc(S(=O)c2cccc(N)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-b5f73f3ea0a54afca47617c9e6b59c43
Cc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1.N>>Cc1cc(C)cc(S(=O)(=O)c2cccc(N)c2C#N)c1
CCOC(=O)C.CC=1C=C(C=C(C1)C)S(=O)(=O)C1=C(C#N)C(=CC=C1)F.N>>NC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC(=C1)C)C
F[c:15]1[cH:14][cH:13][cH:12][c:11]([S:8]([c:7]2[cH:6][c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:20]2)(=[O:9])=[O:10])[c:17]1[C:18]#[N:19].[NH3:16]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7]([S:8](=[O:9])(=[O:10])[c:11]2[cH:12][cH:13][cH:14][c:15]([NH2:16])[c:17]2[C:18]#[N:19])[cH:20]1
Cc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1.N
Cc1cc(C)cc(S(=O)(=O)c2cccc(N)c2C#N)c1
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
5cea7b75c7f95cc50fd74029efa1cddce51f01200160afa4aaecfa45e52a1621
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
O=S(=O)(c1ccccc1)c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[NH3;D0;+0:8]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[NH2;D1;+0:8]):[c:2]:[c:3]
57.5
[{"value": 56.0, "product": "NC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC(=C1)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 57.5, "product": "NC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC(=C1)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-78
CELSIUS
24
HOUR
2-[(3,5-Dimethylphenyl)sulfonyl]-6-fluorobenzonitrile (Example 20) (0.5 g 1.7 mmol) was dissolved in 80 ml of methanol and chilled to -78° C. Condensed ammonia (20 ml, 15.4 g, 905 mmol) was added and the mixture was heated to150° C. in a sealed Parr bomb for 24 h. Chromatography on silica gel (flash; Hex/EtOAc 1:1) pro...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HF
CO
-78
24
Cc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1.N>CO>Cc1cc(C)cc(S(=O)(=O)c2cccc(N)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6c9f5721435e410ba7c84870a32cbc44
COc1cc(C)cc(Br)c1.N#Cc1c(F)cccc1F.[S]>>COc1cc(C)cc(Sc2cccc(F)c2C#N)c1
FC1=C(C#N)C(=CC=C1)F.CS(=O)C.BrC=1C=C(C=C(C1)OC)C.[Li]C(C)CC.[S]>>FC1=C(C#N)C(=CC=C1)SC1=CC(=CC(=C1)OC)C
Br[c:8]1[cH:7][c:5]([CH3:6])[cH:4][c:3]([O:2][CH3:1])[cH:19]1.F[c:10]1[cH:11][cH:12][cH:13][c:14]([F:15])[c:16]1[C:17]#[N:18].[S:9]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH3:6])[cH:7][c:8]([S:9][c:10]2[cH:11][cH:12][cH:13][c:14]([F:15])[c:16]2[C:17]#[N:18])[cH:19]1
COc1cc(C)cc(Br)c1.N#Cc1c(F)cccc1F.[S]
COc1cc(C)cc(Sc2cccc(F)c2C#N)c1
null
null
C1CCOC1.O.C(=O)=O.CC(=O)C
Heteroatom Alkylation and Arylation
OtherReaction
d40080b381033c26189f34d56f4f0aa776c9f43bbed3a9779aed3a120ca17904
204c5e15c927a46727388dfb8648dd74e8e697ddbafa15dfb583665a12d53930
c1ccc(Sc2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].F-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9](-[C:10]#[N;D1;H0:11]):[c:12].[S;H0;D0;+0:13]>>[N;D1;H0:11]#[C:10]-[c:9](:[c:12]):[c;H0;D3;+0:6](-[S;H0;D2;+0:13]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]):[c:7]:[c:8]
null
[]
null
null
20
MINUTE
A solution of 1 g (0.005 mol) of 3-bromo-5-methoxytoluene in 10 mL of freshly distilled THF was cooled in dry ice/acetone and stirred under a N2 atmosphere. To this was added dropwise via a syringe 8.46 mL (0.011 mol) of sec-BuLi (1.3M in cyclohexane). The resultant mixture was stirred for 10 min after which 0.19 g of ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide
Monosulfide
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
Br-
C1CCOC1.O.C(=O)=O.CC(=O)C
null
0.333333
COc1cc(C)cc(Br)c1.N#Cc1c(F)cccc1F.[S]>C1CCOC1.O.C(=O)=O.CC(=O)C>COc1cc(C)cc(Sc2cccc(F)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1a88c0d5212446d3b4c2d1662ded1557
COc1cc(C)cc(Sc2cccc(F)c2C#N)c1.N>>COc1cc(C)cc(Sc2cccc(N)c2C#N)c1
FC1=C(C#N)C(=CC=C1)SC1=CC(=CC(=C1)OC)C.N>>NC1=C(C#N)C(=CC=C1)SC1=CC(=CC(=C1)OC)C
F[c:14]1[cH:13][cH:12][cH:11][c:10]([S:9][c:8]2[cH:7][c:5]([CH3:6])[cH:4][c:3]([O:2][CH3:1])[cH:19]2)[c:16]1[C:17]#[N:18].[NH3:15]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH3:6])[cH:7][c:8]([S:9][c:10]2[cH:11][cH:12][cH:13][c:14]([NH2:15])[c:16]2[C:17]#[N:18])[cH:19]1
COc1cc(C)cc(Sc2cccc(F)c2C#N)c1.N
COc1cc(C)cc(Sc2cccc(N)c2C#N)c1
null
null
C(C)O.C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
5cea7b75c7f95cc50fd74029efa1cddce51f01200160afa4aaecfa45e52a1621
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
c1ccc(Sc2ccccc2)cc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[NH3;D0;+0:8]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[NH2;D1;+0:8]):[c:2]:[c:3]
null
[]
145
CELSIUS
null
null
A solution of 0.1 g (0.00037 mol) of 2-fluoro-6-[(3-methyl-5-methoxyphenyl)thio]benzonitrile (Example 23) in 10 mL of absolute ethanol and ca. 2 mL of THF was saturated with ammonia. The resultant solution was sealed in a glass-lined Parr bomb and heated to 145° C. for 48 h. The solvent was removed in vacuo. 20 mL of 1...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HF
C(C)O.C1CCOC1
145
null
COc1cc(C)cc(Sc2cccc(F)c2C#N)c1.N>C(C)O.C1CCOC1>COc1cc(C)cc(Sc2cccc(N)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-b52dd58a1564476b8012385c8b071efd
COc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1.N>>COc1cc(C)cc(S(=O)(=O)c2cccc(N)c2C#N)c1
FC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC(=C1)OC)C.N>>NC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC(=C1)OC)C
F[c:16]1[cH:15][cH:14][cH:13][c:12]([S:9]([c:8]2[cH:7][c:5]([CH3:6])[cH:4][c:3]([O:2][CH3:1])[cH:21]2)(=[O:10])=[O:11])[c:18]1[C:19]#[N:20].[NH3:17]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH3:6])[cH:7][c:8]([S:9](=[O:10])(=[O:11])[c:12]2[cH:13][cH:14][cH:15][c:16]([NH2:17])[c:18]2[C:19]#[N:20])[cH:21]1
COc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1.N
COc1cc(C)cc(S(=O)(=O)c2cccc(N)c2C#N)c1
null
null
C(C)O.C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
5cea7b75c7f95cc50fd74029efa1cddce51f01200160afa4aaecfa45e52a1621
c5668f64a1395fa45312378ed819baaeafc354cdb673b20226ea2853ed14db5d
O=S(=O)(c1ccccc1)c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[C:5]#[N;D1;H0:6]):[c:7].[NH3;D0;+0:8]>>[N;D1;H0:6]#[C:5]-[c:4](:[c:7]):[c;H0;D3;+0:1](-[NH2;D1;+0:8]):[c:2]:[c:3]
34
[{"value": 34.0, "product": "NC1=C(C#N)C(=CC=C1)S(=O)(=O)C1=CC(=CC(=C1)OC)C", "details": "PERCENTYIELD", "is_desired": false}]
130
CELSIUS
null
null
A solution of 0.3 g (0.00098 mol) of 2-fluoro-6-[(3-methyl-5-methoxyphenyl)sulfonyl]benzonitrile (Example 25) in 10 mL of absolute ethanol and ca. 2 mL of THF was saturated with ammonia. The resultant solution was sealed in a glass-lined Parr bomb and heated to 130° C. for 4 h. The solvent was removed in vacuo. 20 mL o...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Primary amine
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HF
C(C)O.C1CCOC1
130
null
COc1cc(C)cc(S(=O)(=O)c2cccc(F)c2C#N)c1.N>C(C)O.C1CCOC1>COc1cc(C)cc(S(=O)(=O)c2cccc(N)c2C#N)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-57d496f8cfa74e14b0b60ed9b08a5969
CCC(N)C(=O)O.CCOCC.O=S(Cl)Cl>>CCOC(=O)C(N)CC.Cl
NC(C(=O)O)CC.S(=O)(Cl)Cl.C(C)OCC>>Cl.NC(C(=O)OCC)CC
[OH:3][C:4](=[O:5])[CH:6]([NH2:7])[CH2:8][CH3:9].CCO[CH2:2][CH3:1].O=S(Cl)[Cl:10]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([NH2:7])[CH2:8][CH3:9].[ClH:10]
CCC(N)C(=O)O.CCOCC.O=S(Cl)Cl
CCOC(=O)C(N)CC.Cl
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
51b8a6656c0a2b883c9ef3d6e10f16e7a23403a54025d10a356d536fd60cd751
c9da2d501363e26e3362b4d92445c316ae4db0a7128a4caa823650c7a4fa5893
null
C-C-O-[CH2;D2;+0:1]-[C;D1;H3:2].Cl-S(=O)-[Cl;H0;D1;+0:3].[C:4]-[C:5](=[O;D1;H0:6])-[OH;D1;+0:7]>>[C:4]-[C:5](=[O;D1;H0:6])-[O;H0;D2;+0:7]-[CH2;D2;+0:1]-[C;D1;H3:2].[ClH;D0;+0:3]
null
[]
0
CELSIUS
8
HOUR
A slurry of 2-aminobutyric acid (100 g, Aldrich) in absolute ethanol (300 ml) was stirred under nitrogen at 0° C. and thionyl chloride (120.8 g) was added dropwise. The reaction was stirred overnight at 0° C. and then gradually warmed to room temperature. The resulting white slurry was heated under reflux for 3 hours, ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ether
Ester
null
null
null
HCl
C(C)O
0
8
CCC(N)C(=O)O.CCOCC.O=S(Cl)Cl>C(C)O>CCOC(=O)C(N)CC.Cl
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-968da5d345074707bd8ae7f036b4987e
CCOC(=O)C(N)CC.O=Cc1ccccc1>>CCOC(=O)C(CC)N=Cc1ccccc1
C(C1=CC=CC=C1)=O.Cl.NC(C(=O)OCC)CC.S(=O)(=O)([O-])[O-].[Mg+2].C(C)N(CC)CC>>C(C1=CC=CC=C1)=NC(C(=O)OCC)CC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][CH3:8])[NH2:9].O=[CH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][CH3:8])[N:9]=[CH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
CCOC(=O)C(N)CC.O=Cc1ccccc1
CCOC(=O)C(CC)N=Cc1ccccc1
null
null
ClCCl
Heteroatom Alkylation and Arylation
Addition of primary amines to aldehydes/thiocarbonyls
d409dfd3247abb6c1b1364aec380d25720f21e374fd2124063f2d2ce54d31c4f
9b341044a5a058244685b0b956d33f593ccdcd7346fa1d8d7b98a302fd35b8a2
c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[C:9](-[C:10])-[NH2;D1;+0:11]>>[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[C:9](-[C:10])-[N;H0;D2;+0:11]=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]
88.9
[{"value": 88.9, "product": "C(C1=CC=CC=C1)=NC(C(=O)OCC)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
A solution of the product from step (a) (149.6 g), magnesium sulphate (74.3 g), and triethylamine (246 ml) in dichloromethane (1500 ml) was stirred at room temperature under nitrogen and benzaldehyde (94.9 g, Aldrich) was added dropwise. The mixture was stirred at room temperature for 3 hours then filtered. The filtrat...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine
Substituted imine
null
null
c1ccccc1
HO-
ClCCl
null
3
CCOC(=O)C(N)CC.O=Cc1ccccc1>ClCCl>CCOC(=O)C(CC)N=Cc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8bc8a5b260b5493c8773ed6d142bea7c
CC=CCC(N)(CC)C(=O)OCC>>CC=CCC(N)(CC)CO
[OH-].[Na+].NC(C(=O)OCC)(CC=CC)CC.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>NC(CO)(CC=CC)CC
CCO[C:9]([C:5]([CH2:4][CH:3]=[CH:2][CH3:1])([NH2:6])[CH2:7][CH3:8])=[O:10]>>[CH3:1][CH:2]=[CH:3][CH2:4][C:5]([NH2:6])([CH2:7][CH3:8])[CH2:9][OH:10]
CC=CCC(N)(CC)C(=O)OCC
CC=CCC(N)(CC)CO
null
null
C1CCOC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
null
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[C:3](-[C:4])(-[N;D1;H2:5])-[C:6]-[C:7]=[C:8]>>[C:8]=[C:7]-[C:6]-[C:3](-[C:4])(-[N;D1;H2:5])-[CH2;D2;+0:1]-[OH;D1;+0:2]
32.5
[{"value": 32.5, "product": "NC(CO)(CC=CC)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A solution of the product from step (d) (116.7 g) in THF (100 ml) was added to a 1M solution of lithium aluminium hydride in THF (800 ml) at about 0° C. When addition was complete, the mixture was stirred overnight at room temperature, then 50% w/v aqu. NaOH (200 ml) was added. The organic phase was separated, washed w...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
null
HO-
C1CCOC1
null
8
CC=CCC(N)(CC)C(=O)OCC>C1CCOC1>CC=CCC(N)(CC)CO
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-031db419b85e49eb8266022d09028e45
CC=CCC(N)(CC)CO>>CC=CCC1(CC)CN1
ClS(=O)(=O)O.NC(CO)(CC=CC)CC>>C(C=CC)C1(NC1)CC
O[CH2:8][C:5]([CH2:4][CH:3]=[CH:2][CH3:1])([CH2:6][CH3:7])[NH2:9]>>[CH3:1][CH:2]=[CH:3][CH2:4][C:5]1([CH2:6][CH3:7])[CH2:8][NH:9]1
CC=CCC(N)(CC)CO
CC=CCC1(CC)CN1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
2f512f4c744a197f9864da73637475e2ab4d1fc6062fe9117a472495e3ed9f33
405fc0d288d595940df82750271ed5f4125713ca8b676b8ed83063765fec7c50
C1CN1
O-[CH2;D2;+0:1]-[C:2](-[C:3])(-[NH2;D1;+0:4])-[C:5]-[C:6]=[C:7]>>[C:7]=[C:6]-[C:5]-[C:2]1(-[C:3])-[CH2;D2;+0:1]-[NH;D2;+0:4]-1
57
[{"value": 57.0, "product": "C(C=CC)C1(NC1)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Chlorosulphonic acid (18 mL) was added to a solution of the product from step (e) (32.3 g) in acetonitrile (100 ml) at least 9° C. When addition was complete, the mixture was warmed to room temperature. The resulting crystals were filtered off, washed with acetonitrile/pet. ether, dried, taken up in a mixture of 50% w/...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Primary amine
Secondary amine
null
C1CN1
C1CN1
HO-
C(C)#N
null
null
CC=CCC(N)(CC)CO>C(C)#N>CC=CCC1(CC)CN1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-70a686d8594848a0be625406e5a5cefa
CCC(N)(CO)CO.CCO>>CCN1C(=O)OCC1CO
NC(CO)(CO)CC.C(OCC)(OCC)=O.CCO>>C(C)N1C(OCC1CO)=O
C[CH2:7][C:8](CO)([NH2:3])[CH2:9][OH:10].O[CH2:2][CH3:1]>>[CH3:1][CH2:2][N:3]1[C:4](=[O:5])[O:6][CH2:7][CH:8]1[CH2:9][OH:10]
CCC(N)(CO)CO.CCO
CCN1C(=O)OCC1CO
null
C[O-].[Na+]
null
Heteroatom Alkylation and Arylation
OtherReaction
121a8d904936bec16350b8eebf12af85b76bb2c1f851c4c39d775e2c2fc4c968
70fae35b1445ca2d187982b205c3f1487be400228313b6151d1080f84e72b95e
O=C1NCCO1
C-[CH2;D2;+0:1]-[C;H0;D4;+0:2](-[NH2;D1;+0:3])(-C-O)-[C:4]-[O;D1;H1:5].O-[CH2;D2;+0:6]-[C;D1;H3:7]>>[C;D1;H3:7]-[CH2;D2;+0:6]-[N;H0;D3;+0:3]1-[C:8](=[O;D1;H0:9])-[#8:10]-[CH2;D2;+0:1]-[CH;D3;+0:2]-1-[C:4]-[O;D1;H1:5]
null
[]
null
null
null
null
Sodium methoxide (2.2 g, Aldrich) was added to a solution of 2-amino-2-ethyl-1,3-propanediol (100.0 g, Aldrich) and diethyl carbonate (169.0 g, Aldrich) This solution was refluxed in a Dean Stark apparatus until no more EtOH was collected. The reaction mixture was cooled, added acetone (200 ml) and allowed to stand ove...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Primary alcohol.Primary amine
Carbamic ester.Ether
null
C1COC[NH]1
C1COC[NH]1
HO-
C[O-].[Na+]
null
null
CCC(N)(CO)CO.CCO>C[O-].[Na+]>CCN1C(=O)OCC1CO
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-85a305aeebfc4263a0d5dfa4da2ff2f2
CCN1C(=O)OCC1CO.Cc1ccc(S(=O)(=O)Cl)cc1>>CCC1(COS(=O)(=O)c2ccc(C)cc2)COC(=O)N1
Cl.N1=CC=CC=C1.S(=O)(=O)(C1=CC=C(C)C=C1)Cl.C(C)N1C(OCC1CO)=O>>C(C)C1(NC(OC1)=O)COS(=O)(=O)C1=CC=C(C)C=C1
[CH3:1][CH2:2][N:20]1[CH:3]([CH2:4][OH:5])[CH2:16][O:17][C:18]1=[O:19].Cl[S:6](=[O:7])(=[O:8])[c:9]1[cH:10][cH:11][c:12]([CH3:13])[cH:14][cH:15]1>>[CH3:1][CH2:2][C:3]1([CH2:4][O:5][S:6](=[O:7])(=[O:8])[c:9]2[cH:10][cH:11][c:12]([CH3:13])[cH:14][cH:15]2)[CH2:16][O:17][C:18](=[O:19])[NH:20]1
CCN1C(=O)OCC1CO.Cc1ccc(S(=O)(=O)Cl)cc1
CCC1(COS(=O)(=O)c2ccc(C)cc2)COC(=O)N1
null
null
[Cl-].[Na+].O
Acylation
OtherReaction
2e658918820e0aff0c94124acfe4b050c7bb3a642a4c42bb6e5512913bf1e286
7b9c64df079876ee957c060f58afdc2308aed15454df820ab7c4cc2d6b7661b2
O=C1NC(COS(=O)(=O)c2ccccc2)CO1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[C;D1;H3:7]-[CH2;D2;+0:8]-[N;H0;D3;+0:9]1-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]-[CH;D3;+0:14]-1-[C:15]-[OH;D1;+0:16]>>[C;D1;H3:7]-[CH2;D2;+0:8]-[C;H0;D4;+0:14]1(-[C:15]-[O;H0;D2;+0:16]-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6])-[C:13]...
null
[]
null
null
6
HOUR
Tosyl chloride (142.2 g, Aldrich) was added to an ice-chilled solution of the product from step (a) (102.7 g) dissolved in pyridine (175 ml. Aldrich). The reaction mixture was stirred at ice bath temperature for six hours, then allowed to come to room temperature. The heterogeneous mixture was added to 1500 ml of a sol...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Carbamic ester.Primary alcohol.Sulfonyl halide
Tosylate.Carbamic ester
C1COC[NH]1
C1COCN1
c1ccccc1.C1COCN1
HCl
[Cl-].[Na+].O
null
6
CCN1C(=O)OCC1CO.Cc1ccc(S(=O)(=O)Cl)cc1>[Cl-].[Na+].O>CCC1(COS(=O)(=O)c2ccc(C)cc2)COC(=O)N1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-05670d53f7f64813b11aec885e767cda
FC(F)(F)CCI.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>FC(F)(F)CC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[I-]
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.FC(CCI)(F)F>>[I-].FC(CC[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)(F)F
[F:1][C:2]([F:3])([F:4])[CH2:5][CH2:6][I:26].[P: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)[c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1>>[F:1][C:2]([F:3])([F:4])[CH2:5][CH2:6][P+: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)[c:20...
FC(F)(F)CCI.c1ccc(P(c2ccccc2)c2ccccc2)cc1
FC(F)(F)CC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[I-]
null
null
null
Functional Group Interconversion
OtherReaction
72a5231b07f184f0ef4a0648badd4176f521b95f1ba3340a0f90d8894af47260
47a659f5704a5b7ca1b92ff731f18f109c6bde1d45152a3a393eefbd10265508
c1ccc([PH+](c2ccccc2)c2ccccc2)cc1
[F;D1;H0:1]-[C:2](-[F;D1;H0:3])(-[F;D1;H0:4])-[C:5]-[CH2;D2;+0:6]-[I;H0;D1;+0:7].[c:8]:[c:9](-[P;H0;D3;+0:10](-[c:11](:[c:12]):[c:13])-[c:14](:[c:15]):[c:16]):[c:17]>>[F;D1;H0:1]-[C:2](-[F;D1;H0:3])(-[F;D1;H0:4])-[C:5]-[CH2;D2;+0:6]-[P+;H0;D4:10](-[c:11](:[c:12]):[c:13])(-[c:14](:[c:15]):[c:16])-[c:9](:[c:8]):[c:17].[I...
76.5
[{"value": 76.5, "product": "[I-].FC(CC[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of triphenylphosphine (Aldrich, 11.7 g) and 3,3,3-trifluoropropyl iodid (Lancaster, 10 g) was vigorously refluxed in xylenes (75 mL) for 2 days. The solid which formed was filtered and washed with xylenes then air dried to yield a white solid (16.6 g). 1H NMR and elemental analysis are consistent with the pr...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
null
null
c1ccccc1.c1ccccc1.c1ccccc1
null
null
null
null
FC(F)(F)CCI.c1ccc(P(c2ccccc2)c2ccccc2)cc1>>FC(F)(F)CC[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[I-]
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a4b47970bbbd496493b0100b353ff70e
N#Cc1ccc(CBr)cc1.[N-]=[N+]=[N-]>>N#Cc1ccc(CN=[N+]=[N-])cc1
[N-]=[N+]=[N-].[Na+].C(#N)C1=CC=C(CBr)C=C1>>C(#N)C1=CC=C(CN=[N+]=[N-])C=C1
Br[CH2:7][c:6]1[cH:5][cH:4][c:3]([C:2]#[N:1])[cH:12][cH:11]1.[N-:8]=[N+:9]=[N-:10]>>[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][N:8]=[N+:9]=[N-:10])[cH:11][cH:12]1
N#Cc1ccc(CBr)cc1.[N-]=[N+]=[N-]
N#Cc1ccc(CN=[N+]=[N-])cc1
null
null
CN(C)C=O.C1(=CC=CC=C1)C.O
Heteroatom Alkylation and Arylation
OtherReaction
4b07a4c2a14d792a37e78a751619e60b15c60cbff0bebae1109754fb52d84cbb
2d41632f7225d65cdc2ad8562dfb28f3f5a017f92040ed4ccafbb8154954c8fe
c1ccccc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[N-;H0;D1:5]=[#7;+:6]=[N;-;D1;H0:7]>>[N;-;D1;H0:7]=[#7;+:6]=[N;H0;D2;+0:5]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
A solution of 20.23 g (0.31 mol) sodium azide in 50 ml water was added to 49.15 g (251 mmol) 4-cyanobenzyl bromide in 200 ml DMF at ambient temperature. An exothermic reaction took place and after 1.5 h the reaction mixture was diluted with 200 ml toluene(caution: In order to avoid separation of potentially explosive a...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Azide
null
null
c1ccccc1
Br-
CN(C)C=O.C1(=CC=CC=C1)C.O
null
null
N#Cc1ccc(CBr)cc1.[N-]=[N+]=[N-]>CN(C)C=O.C1(=CC=CC=C1)C.O>N#Cc1ccc(CN=[N+]=[N-])cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8c0bae38a8294d0e9674fa88542622fe
O=C(Cl)OCc1ccccc1.[N-]=[N+]=NCc1ccc(C(=N)N)cc1>>[N-]=[N+]=NCc1ccc(C(=N)NC(=O)OCc2ccccc2)cc1
ClC(=O)OCC1=CC=CC=C1.C(N)(=N)C1=CC=C(CN=[N+]=[N-])C=C1.C(C)N(CC)CC.Cl.ClC(=O)OCC1=CC=CC=C1>>C(C1=CC=CC=C1)OC(=O)NC(=N)C1=CC=C(CN=[N+]=[N-])C=C1
Cl[C:12](=[O:13])[O:14][CH2:15][c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1.[N-:1]=[N+:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([C:9](=[NH:10])[NH2:11])[cH:22][cH:23]1>>[N-:1]=[N+:2]=[N:3][CH2:4][c:5]1[cH:6][cH:7][c:8]([C:9](=[NH:10])[NH:11][C:12](=[O:13])[O:14][CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[cH:22][c...
O=C(Cl)OCc1ccccc1.[N-]=[N+]=NCc1ccc(C(=N)N)cc1
[N-]=[N+]=NCc1ccc(C(=N)NC(=O)OCc2ccccc2)cc1
null
null
C(Cl)Cl.O
Protection
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
038720aa61a7efa0f2a9ee6f2e0adf63a9ffdc2be4697c11a6215baef34f97b2
205f353513ce9506ab61831799da8fb73ec2ef5cfa927664496d3ce72c438860
N=C(NC(=O)OCc1ccccc1)c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C:4].[N;D1;H1:5]=[C:6](-[NH2;D1;+0:7])-[c:8]>>[C:4]-[#8:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:7]-[C:6](=[N;D1;H1:5])-[c:8]
null
[]
null
null
30
MINUTE
The crystals from (ii) above were dissolved in 500 ml methylene chloride and the resulting solution was dried (K2CO3), filtered and 27 ml (194 mmol) triethyl amine was added. 25 ml Benzyl chloroformate was slowly added to the stirred solution while the reaction mixture was cooled in an ice bath. After 30 minutes an add...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether.Primary amine
Carbamic ester
null
null
c1ccccc1.c1ccccc1
HCl
C(Cl)Cl.O
null
0.5
O=C(Cl)OCc1ccccc1.[N-]=[N+]=NCc1ccc(C(=N)N)cc1>C(Cl)Cl.O>[N-]=[N+]=NCc1ccc(C(=N)NC(=O)OCc2ccccc2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-91be128b9742407397cb2ab366a4130b
[N-]=[N+]=NCc1ccc(C(=N)NC(=O)OCc2ccccc2)cc1>>N=C(NC(=O)OCc1ccccc1)c1ccc(CN)cc1
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(C1=CC=CC=C1)OC(=O)NC(=N)C1=CC=C(CN=[N+]=[N-])C=C1.C(C1=CC=CC=C1)OC(=O)NC(=N)C1=CC=C(CN=[N+]=[N-])C=C1.C(#N)C(C1=CC=CC=C1)Br>>NCC1=CC=C(C=C1)C(NC(=O)OCC1=CC=CC=C1)=N
[N-]=[N+]=[N:19][CH2:18][c:17]1[cH:16][cH:15][c:14]([C:2](=[NH:1])[NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[cH:21][cH:20]1>>[NH:1]=[C:2]([NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1)[c:14]1[cH:15][cH:16][c:17]([CH2:18][NH2:19])[cH:20][cH:21]1
[N-]=[N+]=NCc1ccc(C(=N)NC(=O)OCc2ccccc2)cc1
N=C(NC(=O)OCc1ccccc1)c1ccc(CN)cc1
null
null
C1CCOC1
Reduction
Azide to amine reduction (Staudinger)
4c9e4990dae2bb965dec06bd45e318560989ee3681b61e443f7aa363b7cfa222
cd009d687d606bf351eac9390a176d16be38f2c8216a599b398641009c215027
N=C(NC(=O)OCc1ccccc1)c1ccccc1
[N-]=[N+]=[N;H0;D2;+0:1]-[C:2]-[c:3]>>[NH2;D1;+0:1]-[C:2]-[c:3]
null
[]
null
null
null
null
26.3 g (100 mmol) triphenylphosphine was added at room temperature to the 4-(benzyloxycarbonylamidino) benzyl azide from (iii) above dissolved in 160 ml THF. After 16 h an additional 6.6 g (25 mmol) triphenylphosphine was added and the solution was allowed to stand for 4 h before removal of the solvent in vacuo. The re...
10.6084/m9.figshare.5104873.v1
null
Azide
Primary amine
null
null
c1ccccc1.c1ccccc1
Other
C1CCOC1
null
null
[N-]=[N+]=NCc1ccc(C(=N)NC(=O)OCc2ccccc2)cc1>C1CCOC1>N=C(NC(=O)OCc1ccccc1)c1ccc(CN)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0b5d6ed5aa3144caa92cff165e2d40f8
CC(C)(C)OC(=O)NCC1CCNCC1.CSC(=N)NC(=O)OCc1ccccc1>>CC(C)(C)OC(=O)NCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1
C(C)(C)(C)OC(=O)NCC1CCNCC1.C(C1=CC=CC=C1)OC(=O)NC(SC)=N>>C(C)(C)(C)OC(=O)NCC1CCN(CC1)C(NC(=O)OCC1=CC=CC=C1)=N
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH:10]1[CH2:11][CH2:12][NH:13][CH2:27][CH2:28]1.CS[C:14](=[NH:15])[NH:16][C:17](=[O:18])[O:19][CH2:20][c:21]1[cH:22][cH:23][cH:24][cH:25][cH:26]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH:10]1[CH2:11][CH2:12][N:13]([C:14](=[NH:15])[NH...
CC(C)(C)OC(=O)NCC1CCNCC1.CSC(=N)NC(=O)OCc1ccccc1
CC(C)(C)OC(=O)NCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
1b47623bd99949b4cf4f2fee4856128f888eea2f61ec86d31845b541c33c66e1
f5aa33108984aad43441754644c214239e577e2035dc027b4aa13ab85821a21b
N=C(NC(=O)OCc1ccccc1)N1CCCCC1
C-S-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[C:4](-[#8:5])=[O;D1;H0:6].[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]>>[#8:5]-[C:4](=[O;D1;H0:6])-[#7:3]-[C;H0;D3;+0:1](=[N;D1;H1:2])-[N;H0;D3;+0:9](-[C:8]-[C:7])-[C:10]-[C:11]
37
[{"value": 37.0, "product": "C(C)(C)(C)OC(=O)NCC1CCN(CC1)C(NC(=O)OCC1=CC=CC=C1)=N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 36.7, "product": "C(C)(C)(C)OC(=O)NCC1CCN(CC1)C(NC(=O)OCC1=CC=CC=C1)=N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
DAY
7.8 g (36.4 mmole) of 4-(N-tert-butyloxycarbonylaminomethyl) piperidine and 8.98 g (40 mmole) of N-benzyloxycarbonyl-S-methylisothiourea was mixed in 25 mL ethanol. The mixture was heated at 60°-70° C. for six hours and left at room temperature for two days. The solvent was evaporated and the residue was dissolved in C...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Monosulfide
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccccc1
Other
C(C)O
null
48
CC(C)(C)OC(=O)NCC1CCNCC1.CSC(=N)NC(=O)OCc1ccccc1>C(C)O>CC(C)(C)OC(=O)NCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-38cb457f7729445685e412a4fffa8894
CSC(=N)NC(=O)OCc1ccccc1.OCCC1CCNCC1>>N=C(NC(=O)OCc1ccccc1)N1CCC(CCO)CC1
OCCC1CCNCC1.C(C1=CC=CC=C1)OC(=O)NC(SC)=N>>C(C1=CC=CC=C1)OC(=O)NC(=N)N1CCC(CC1)CCO
CS[C:2](=[NH:1])[NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1.[NH:14]1[CH2:15][CH2:16][CH:17]([CH2:18][CH2:19][OH:20])[CH2:21][CH2:22]1>>[NH:1]=[C:2]([NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1)[N:14]1[CH2:15][CH2:16][CH:17]([CH2:18][CH2:19][OH:20])[CH2:21][CH2:22...
CSC(=N)NC(=O)OCc1ccccc1.OCCC1CCNCC1
N=C(NC(=O)OCc1ccccc1)N1CCC(CCO)CC1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
1b47623bd99949b4cf4f2fee4856128f888eea2f61ec86d31845b541c33c66e1
f5aa33108984aad43441754644c214239e577e2035dc027b4aa13ab85821a21b
N=C(NC(=O)OCc1ccccc1)N1CCCCC1
C-S-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[C:4](-[#8:5])=[O;D1;H0:6].[C:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]>>[#8:5]-[C:4](=[O;D1;H0:6])-[#7:3]-[C;H0;D3;+0:1](=[N;D1;H1:2])-[N;H0;D3;+0:9](-[C:8]-[C:7])-[C:10]-[C:11]
41
[{"value": 41.0, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CCC(CC1)CCO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 40.9, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CCC(CC1)CCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 6.2 g (0.028 mol) of 4-hydroxyethyl piperidine and 3.6 g (0.028 mol) of N-benzyloxycarbonyl-S-methyl isothiourea in 50 ml of acetonitrile was refluxed overnight. Evaporation and flash chromatography on silica gel with ethyl acetate gave 3.5 g (41%) of the title compound. Conditions: See reaction.notes.proc...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Monosulfide
Tertiary amine
C1CCNCC1
C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1
Other
C(C)#N
null
null
CSC(=N)NC(=O)OCc1ccccc1.OCCC1CCNCC1>C(C)#N>N=C(NC(=O)OCc1ccccc1)N1CCC(CCO)CC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d3631dc5ac684ec9b01dd5b9b7ce5987
CS(=O)(=O)OCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1.[N-]=[N+]=[N-]>>[N-]=[N+]=NCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1
C(C1=CC=CC=C1)OC(=O)NC(=N)N1CCC(CC1)CCOS(=O)(=O)C.[N-]=[N+]=[N-].[Na+].O>>N(=[N+]=[N-])CCC1CCN(CC1)C(NC(=O)OCC1=CC=CC=C1)=N
CS(=O)(=O)O[CH2:4][CH2:5][CH:6]1[CH2:7][CH2:8][N:9]([C:10](=[NH:11])[NH: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][CH2:24]1.[N-:1]=[N+:2]=[N-:3]>>[N-:1]=[N+:2]=[N:3][CH2:4][CH2:5][CH:6]1[CH2:7][CH2:8][N:9]([C:10](=[NH:11])[NH:12][C:13](=[O:14])[O:15][CH2:16][c:17]2[cH:18][cH:19...
CS(=O)(=O)OCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1.[N-]=[N+]=[N-]
[N-]=[N+]=NCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
341eb24906c58cd9cfdeec13febaf0724780d7854e6b6d7ec703218c4bcbe27b
5f2cb2b9819a73a6855f5277f7fe9d5ce3871340baaebb59d42e38e1ca145c0a
N=C(NC(=O)OCc1ccccc1)N1CCCCC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2]-[C:3].[N-;H0;D1:4]=[#7;+:5]=[N;-;D1;H0:6]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D2;+0:4]=[#7;+:5]=[N;-;D1;H0:6]
null
[]
100
CELSIUS
null
null
In 100 ml of dimethylformamide was dissolve (0.0115 mol) of crude 1-benzyloxycarbonylamidino-4-mesyloxyethyl piperidine and 4.5 g (0.069 mol) of sodium azide was added. The mixture was heated at 100° C. for 2.5 h. It was then poured into water and extracted with ethyl acetate three times. The combined organic phase was...
10.6084/m9.figshare.5104873.v1
null
Mesylate
Azide
null
null
C1CC[NH]CC1.c1ccccc1
MsOH.HO-
CN(C=O)C
100
null
CS(=O)(=O)OCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1.[N-]=[N+]=[N-]>CN(C=O)C>[N-]=[N+]=NCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2080a877db5f4bf4b20e375ca34bad46
[N-]=[N+]=NCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1>>N=C(NC(=O)OCc1ccccc1)N1CCC(CCN)CC1
Cl.[BH4-].[Na+].N(=[N+]=[N-])CCC1CCN(CC1)C(NC(=O)OCC1=CC=CC=C1)=N>>NCCC1CCN(CC1)C(NC(=O)OCC1=CC=CC=C1)=N
[N-]=[N+]=[N:20][CH2:19][CH2:18][CH:17]1[CH2:16][CH2:15][N:14]([C:2](=[NH:1])[NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[CH2:22][CH2:21]1>>[NH:1]=[C:2]([NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1)[N:14]1[CH2:15][CH2:16][CH:17]([CH2:18][CH2:19][NH2:20])[CH2:21][...
[N-]=[N+]=NCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1
N=C(NC(=O)OCc1ccccc1)N1CCC(CCN)CC1
null
[Pd].[Pd]
O.O1CCCC1
Reduction
Azide to amine reduction (Staudinger)
4c9e4990dae2bb965dec06bd45e318560989ee3681b61e443f7aa363b7cfa222
cd009d687d606bf351eac9390a176d16be38f2c8216a599b398641009c215027
N=C(NC(=O)OCc1ccccc1)N1CCCCC1
[C:1]-[C:2]-[N;H0;D2;+0:3]=[N+]=[N-]>>[C:1]-[C:2]-[NH2;D1;+0:3]
null
[]
null
null
null
null
To 30 ml of water was added 0.40 g of 10% Pd/C. Sodium borohydride, 1.0 g (0.031 mol), was dissolved in 30 ml of water and was added carefully to the stirred and ice-cooled slurry of Pd/C and water. 4-Azidoethyl-1-benzyloxycarbonylamidino piperidine, 2.9 g (8.8 mmol), was dissolved in 80 ml of tetrahydrofurane and this...
10.6084/m9.figshare.5104873.v1
null
Azide
Primary amine
null
null
c1ccccc1.C1CC[NH]CC1
Other
[Pd].[Pd].O.O1CCCC1
null
null
[N-]=[N+]=NCCC1CCN(C(=N)NC(=O)OCc2ccccc2)CC1>[Pd].[Pd].O.O1CCCC1>N=C(NC(=O)OCc1ccccc1)N1CCC(CCN)CC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-66270614c8d046a8af9a342eb13c4b24
COC(=N)NC(=O)OCc1ccccc1.OCC1CCNC1>>N=C(NC(=O)OCc1ccccc1)N1CCC(CO)C1
OCC1CNCC1.C(C1=CC=CC=C1)OC(=O)NC(OC)=N>>C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CO
CO[C:2](=[NH:1])[NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1.[NH:14]1[CH2:15][CH2:16][CH:17]([CH2:18][OH:19])[CH2:20]1>>[NH:1]=[C:2]([NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1)[N:14]1[CH2:15][CH2:16][CH:17]([CH2:18][OH:19])[CH2:20]1
COC(=N)NC(=O)OCc1ccccc1.OCC1CCNC1
N=C(NC(=O)OCc1ccccc1)N1CCC(CO)C1
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
4b0f97014035cf0d99b32a42bcb79ab87c0cd49b39ff30f05a7ff00b27a74c06
f41a0ac1ece338534be38b696cb3541e6003cebbbc2e76e91361a568e6946ab0
N=C(NC(=O)OCc1ccccc1)N1CCCC1
C-O-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[C:4](-[#8:5])=[O;D1;H0:6].[C:7]1-[C:8]-[C:9]-[C:10]-[NH;D2;+0:11]-1>>[#8:5]-[C:4](=[O;D1;H0:6])-[#7:3]-[C;H0;D3;+0:1](=[N;D1;H1:2])-[N;H0;D3;+0:11]1-[C:7]-[C:8]-[C:9]-[C:10]-1
25.2
[{"value": 25.0, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 25.2, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
null
null
1.01 g (0.01 mole) (3RS)-3-hydroxymethyl pyrrolidine and 2.29 g (0.011 mole) N-benzyloxycarbonyl-O-methylisourea was dissolved (the amine not very soluble) in toluene and heated to 60° C. for three hours followed by stirring at room temperature over night. The mixture was evaporated and the 1H-NMR showed that the react...
10.6084/m9.figshare.5104873.v1
null
Ether.Secondary amine
Tertiary amine
C1CCNC1
C1CC[NH]C1
c1ccccc1.C1CC[NH]C1
HO-
C1(=CC=CC=C1)C
60
null
COC(=N)NC(=O)OCc1ccccc1.OCC1CCNC1>C1(=CC=CC=C1)C>N=C(NC(=O)OCc1ccccc1)N1CCC(CO)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-50d2591cf07947e7ab725904f4df96f4
CS(=O)(=O)Cl.N=C(NC(=O)OCc1ccccc1)N1CCC(CO)C1>>CS(=O)(=O)OCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1
CS(=O)(=O)Cl.C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CO.C(C)N(CC)CC>>C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)COS(=O)(=O)C
Cl[S:2]([CH3:1])(=[O:3])=[O:4].[OH:5][CH2:6][CH:7]1[CH2:8][CH2:9][N:10]([C:11](=[NH:12])[NH:13][C:14](=[O:15])[O:16][CH2:17][c:18]2[cH:19][cH:20][cH:21][cH:22][cH:23]2)[CH2:24]1>>[CH3:1][S:2](=[O:3])(=[O:4])[O:5][CH2:6][CH:7]1[CH2:8][CH2:9][N:10]([C:11](=[NH:12])[NH:13][C:14](=[O:15])[O:16][CH2:17][c:18]2[cH:19][cH:20]...
CS(=O)(=O)Cl.N=C(NC(=O)OCc1ccccc1)N1CCC(CO)C1
CS(=O)(=O)OCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1
null
null
C(C)(=O)OCC.CCCCCCC.C(C)OCC
Acylation
Formation of Sulfonic Esters
2fa969eb2c954bb96793348a1b2335ec63fbd290dadec6e3e02295e1768e64cf
cb77b899e4adf980b1def97230ef2861660fd7f9602260ec64747d9afd3a795a
N=C(NC(=O)OCc1ccccc1)N1CCCC1
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]
50
[{"value": 50.0, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)COS(=O)(=O)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 50.0, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)COS(=O)(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
3
HOUR
0.7 g (2.53 mmole) (3RS)-1-(N-benzyloxycarbonylamidino)-3-hydroxymethyl pyrrolidine and 0.70 ml (5.05 mmole) triethylamine was dissolved in 15 ml diethyl ether/CH2Cl2 1/1 and the mixture was cooled to 0° C. 0.25 ml (3.29 mmole) methanesulphonyl chloride in 3 ml diethyl ether was slowly added and the reaction mixture wa...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Sulfonyl halide
Mesylate
null
null
C1CC[NH]C1.c1ccccc1
HCl
C(C)(=O)OCC.CCCCCCC.C(C)OCC
0
3
CS(=O)(=O)Cl.N=C(NC(=O)OCc1ccccc1)N1CCC(CO)C1>C(C)(=O)OCC.CCCCCCC.C(C)OCC>CS(=O)(=O)OCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8f9821df03a7466091a3423b9a248655
CS(=O)(=O)OCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1.[N-]=[N+]=[N-]>>[N-]=[N+]=NCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1
C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)COS(=O)(=O)C.[N-]=[N+]=[N-].[Na+].O>>C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CN=[N+]=[N-]
CS(=O)(=O)O[CH2:4][CH:5]1[CH2:6][CH2:7][N:8]([C:9](=[NH:10])[NH:11][C:12](=[O:13])[O:14][CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[CH2:22]1.[N-:1]=[N+:2]=[N-:3]>>[N-:1]=[N+:2]=[N:3][CH2:4][CH:5]1[CH2:6][CH2:7][N:8]([C:9](=[NH:10])[NH:11][C:12](=[O:13])[O:14][CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)...
CS(=O)(=O)OCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1.[N-]=[N+]=[N-]
[N-]=[N+]=NCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
341eb24906c58cd9cfdeec13febaf0724780d7854e6b6d7ec703218c4bcbe27b
5f2cb2b9819a73a6855f5277f7fe9d5ce3871340baaebb59d42e38e1ca145c0a
N=C(NC(=O)OCc1ccccc1)N1CCCC1
C-S(=O)(=O)-O-[CH2;D2;+0:1]-[C:2](-[C:3])-[C:4]-[#7:5].[N-;H0;D1:6]=[#7;+:7]=[N;-;D1;H0:8]>>[#7:5]-[C:4]-[C:2](-[CH2;D2;+0:1]-[N;H0;D2;+0:6]=[#7;+:7]=[N;-;D1;H0:8])-[C:3]
68.2
[{"value": 68.0, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CN=[N+]=[N-]", "details": "PERCENTYIELD", "is_desired": false}, {"value": 68.2, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CN=[N+]=[N-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
null
null
0.450 g (1.27 mmole) (3RS)-1-(N-benzyloxycarbonylamidino)-3-mesyloxymethyl pyrrolidine and 0.124 g (1.9 mmole) of sodium azide were dissolved in 10 ml dimethylformamide and heated to 60° C. for four hours followed by stirring at room temperature over night. Water was added and the mixture was extracted twice with tolue...
10.6084/m9.figshare.5104873.v1
null
Mesylate
Azide
null
null
C1CC[NH]C1.c1ccccc1
MsOH.HO-
CN(C=O)C
60
null
CS(=O)(=O)OCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1.[N-]=[N+]=[N-]>CN(C=O)C>[N-]=[N+]=NCC1CCN(C(=N)NC(=O)OCc2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1537debbdfcd4c9fb2d97af472b6fc7c
O=S(Cl)Cl.OCC1CCN(Cc2ccccc2)C1>>ClCC1CCN(Cc2ccccc2)C1
C(C1=CC=CC=C1)N1CC(CC1)CO.S(=O)(Cl)Cl>>C(C1=CC=CC=C1)N1CC(CC1)CCl
O=S(Cl)[Cl:1].O[CH2:2][CH: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>>[Cl:1][CH2:2][CH: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
O=S(Cl)Cl.OCC1CCN(Cc2ccccc2)C1
ClCC1CCN(Cc2ccccc2)C1
null
null
C(Cl)(Cl)Cl
Functional Group Interconversion
Alcohol to chloride_SOCl2
bb752b9027dc4488ba075e5955118a819f80cabd751a7497b67c2eeb1db6b071
cbf41c7cf9fe6b47a243b1674d74ed5bf46a151f7f3a71d206e23176e158facf
c1ccc(CN2CCCC2)cc1
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3](-[C:4])-[C:5]-[#7:6]>>[#7:6]-[C:5]-[C:3](-[CH2;D2;+0:2]-[Cl;H0;D1;+0:1])-[C:4]
null
[]
null
null
1
HOUR
To a refluxing solution of 15.3 g (0.08 mole) (3RS)-1-benzyl-3-hydroxymethyl pyrrolidine in 220 ml CHCl3 was slowly added a solution of 330 ml thionyl chloride in 60 ml CHCl3, and the reflux was continued for one hour. The mixture was evaporated and the residue was dissolved in water. Conditions: See reaction.notes.pro...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Primary halide
null
null
C1CC[NH]C1.c1ccccc1
HCl
C(Cl)(Cl)Cl
null
1
O=S(Cl)Cl.OCC1CCN(Cc2ccccc2)C1>C(Cl)(Cl)Cl>ClCC1CCN(Cc2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-56818a6d757b4766865fa51ce27de994
ClCC1CCN(Cc2ccccc2)C1.[C-]#N>>N#CCC1CCN(Cc2ccccc2)C1
C(C1=CC=CC=C1)N1CC(CC1)CCl.[C-]#N.[Na+].O>>C(C1=CC=CC=C1)N1CC(CC1)CC#N
Cl[CH2:3][CH:4]1[CH2:5][CH2:6][N:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1.[N:1]#[C-:2]>>[N:1]#[C:2][CH2:3][CH:4]1[CH2:5][CH2:6][N:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1
ClCC1CCN(Cc2ccccc2)C1.[C-]#N
N#CCC1CCN(Cc2ccccc2)C1
null
null
CS(=O)C
C-C Coupling
OtherReaction
347b040e695b34bb71d78d55beea9c7162795a061d052426f1f803b52c4cbe4d
1dbefa1fc17e03074aa3f6619987f71dfa9a1cb0d61de142a880cd3f05e4f004
c1ccc(CN2CCCC2)cc1
Cl-[CH2;D2;+0:1]-[C:2](-[C:3])-[C:4]-[#7:5].[C-;H0;D1:6]#[N;D1;H0:7]>>[#7:5]-[C:4]-[C:2](-[CH2;D2;+0:1]-[C;H0;D2;+0:6]#[N;D1;H0:7])-[C:3]
92
[{"value": 92.0, "product": "C(C1=CC=CC=C1)N1CC(CC1)CC#N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.7, "product": "C(C1=CC=CC=C1)N1CC(CC1)CC#N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
2
DAY
16.8 g (0.08 mole) (3RS)-1-benzyl-3-chloromethyl pyrrolidine and 5.88 g (0.12 mole) of sodium cyanide was dissolved in 250 ml dimethyl sulfoxide. The mixture was stirred at 60° C. for two days and at room temperature for one week. Water was added and the mixture was extracted three times with ethyl acetate. The combine...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Nitrile
null
null
C1CC[NH]C1.c1ccccc1
Other
CS(=O)C
60
48
ClCC1CCN(Cc2ccccc2)C1.[C-]#N>CS(=O)C>N#CCC1CCN(Cc2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-355bf43961874334b0dd644d901cbbcf
N#CCC1CCN(Cc2ccccc2)C1>>NCCC1CCN(Cc2ccccc2)C1
[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+].O.C(C1=CC=CC=C1)N1CC(CC1)CC#N>>C(C1=CC=CC=C1)N1CC(CC1)CCN
[N:1]#[C:2][CH2:3][CH:4]1[CH2:5][CH2:6][N:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1>>[NH2:1][CH2:2][CH2:3][CH:4]1[CH2:5][CH2:6][N:7]([CH2:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[CH2:15]1
N#CCC1CCN(Cc2ccccc2)C1
NCCC1CCN(Cc2ccccc2)C1
null
null
C(C)OCC
Reduction
Reduction of nitrile to amine
65bec2d9f430701d30dc9fcbe1c5418f3dfa174d67be035c50edfc71895dc9c7
e8d1bc928b94bd4f5bf4b23363ce8f88b1ce7d146ba93829e7b8ad8dbe0007a7
c1ccc(CN2CCCC2)cc1
[C:1]-[C:2]-[C;H0;D2;+0:3]#[N;H0;D1;+0:4]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[NH2;D1;+0:4]
99
[{"value": 99.0, "product": "C(C1=CC=CC=C1)N1CC(CC1)CCN", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.0, "product": "C(C1=CC=CC=C1)N1CC(CC1)CCN", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
14.7 g (0.0734 mole) (3RS)-1-benzyl-3-cyanomethyl pyrrolidine dissolved in 220 ml diethyl ether was slowly added to a slurry of 2.94 g of lithium aluminium hydride in 74 ml diethyl ether under an argon atmosphere. The mixture was stirred over night,and 6 ml water, 18 ml 3.75M NaOH-solution and 6 ml water was added to t...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
C1CC[NH]C1.c1ccccc1
null
C(C)OCC
null
null
N#CCC1CCN(Cc2ccccc2)C1>C(C)OCC>NCCC1CCN(Cc2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2326e4f1e4844936a51646b96ee23d0d
CC(C)(C)OC(=O)NCCC1CCN(Cc2ccccc2)C1>>CC(C)(C)OC(=O)NCCC1CCNC1
C(C1=CC=CC=C1)N1CC(CC1)CCNC(=O)OC(C)(C)C>>C(C)(C)(C)OC(=O)NCCC1CNCC1
c1ccc(C[N:14]2[CH2:13][CH2:12][CH:11]([CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:15]2)cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH:11]1[CH2:12][CH2:13][NH:14][CH2:15]1
CC(C)(C)OC(=O)NCCC1CCN(Cc2ccccc2)C1
CC(C)(C)OC(=O)NCCC1CCNC1
null
[OH-].[OH-].[Pd+2]
C(C)O
Deprotection
Hydrogenolysis of tertiary amines
846a35f8c83fa58d2c714915319a8bc96745602a4dd9ac20dbad14bc1e16a470
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
C1CCNC1
C(-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1)-c1:c:c:c:c:c:1>>[C:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:5]-1
null
[]
null
null
null
null
3.1 g (0.0t mol) (3RS)-1-benzyl-3-(N-tert-butyloxycarbonylaminoethyl) pyrrolidine was hydrogenated at 0.28 MPa over 0.6 g of Pearlman's catalyst (Pd(OH)2) in 40 ml ethanol (95%) over night. After filtration of the catalyst through cellite and evaporation of the solvent 1H-NMR showed that the reaction was not completed....
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.C1CC[NH]C1
C1CCNC1
C1CCNC1
Other
[OH-].[OH-].[Pd+2].C(C)O
null
null
CC(C)(C)OC(=O)NCCC1CCN(Cc2ccccc2)C1>[OH-].[OH-].[Pd+2].C(C)O>CC(C)(C)OC(=O)NCCC1CCNC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d42f48a7d3fc473aba6c5139093935b5
CC(C)(C)OC(=O)NCCC1CCNC1.CSC(=N)NC(=O)OCc1ccccc1>>N=C(NC(=O)OCc1ccccc1)N1CCC(CCN)C1
C(C)(C)(C)OC(=O)NCCC1CNCC1.C(C1=CC=CC=C1)OC(=O)NC(SC)=N.OS(=O)(=O)[O-].[K+]>>C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CCN
CC(C)(C)OC(=O)[NH:20][CH2:19][CH2:18][CH:17]1[CH2:16][CH2:15][NH:14][CH2:21]1.CS[C:2](=[NH:1])[NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1>>[NH:1]=[C:2]([NH:3][C:4](=[O:5])[O:6][CH2:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1)[N:14]1[CH2:15][CH2:16][CH:17]([CH2:18][CH2:19][NH2:20])[CH2:21]1
CC(C)(C)OC(=O)NCCC1CCNC1.CSC(=N)NC(=O)OCc1ccccc1
N=C(NC(=O)OCc1ccccc1)N1CCC(CCN)C1
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
e41463d89a0c3093b9e549b0fd45908e8b91cfc217a44320d33492e3fcab5e4f
403a59c8b6e9766a4301d1da3109f0687a3485a98c4d8eacd70e1f338293189c
N=C(NC(=O)OCc1ccccc1)N1CCCC1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]-[C:4]1-[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-1.C-S-[C;H0;D3;+0:9](=[N;D1;H1:10])-[#7:11]-[C:12](-[#8:13])=[O;D1;H0:14]>>[#8:13]-[C:12](=[O;D1;H0:14])-[#7:11]-[C;H0;D3;+0:9](=[N;D1;H1:10])-[N;H0;D3;+0:7]1-[C:6]-[C:5]-[C:4](-[C:3]-[C:2]-[NH2;D1;+0:1])-[C:8]-1
67.5
[{"value": 51.0, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CCN", "details": "PERCENTYIELD", "is_desired": false}, {"value": 67.5, "product": "C(C1=CC=CC=C1)OC(=O)NC(=N)N1CC(CC1)CCN", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
DAY
2.18 g (0.0102 mole) (3RS)-3-(N-tert-butyloxycarbonylaminoethyl) pyrrolidine and 2.81 g (0.0125 mole) N-benzyloxycarbonyl-S-methylisothiourea was dissolved in 30 ml toluene and heated to 60°-70° C. for eight hours followed by stirring at room temperature for one day. 0.3M KHSO4 -solution was added and the water layer w...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Secondary amine.Monosulfide.Boc
Primary amine.Tertiary amine
C1CCNC1
C1CC[NH]C1
c1ccccc1.C1CC[NH]C1
Other
C1(=CC=CC=C1)C
null
24
CC(C)(C)OC(=O)NCCC1CCNC1.CSC(=N)NC(=O)OCc1ccccc1>C1(=CC=CC=C1)C>N=C(NC(=O)OCc1ccccc1)N1CCC(CCN)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ecbc4c566e744d9b960cfaf350b242df
CC(C)(C)OC(=O)NCC1CN(C(c2ccccc2)c2ccccc2)C1>>CC(C)(C)OC(=O)NCC1CNC1
C(C)(C)(C)OC(=O)NCC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1>>C(C)(C)(C)OC(=O)NCC1CNC1
c1ccc(C(c2ccccc2)[N:12]2[CH2:11][CH:10]([CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:13]2)cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH:10]1[CH2:11][NH:12][CH2:13]1
CC(C)(C)OC(=O)NCC1CN(C(c2ccccc2)c2ccccc2)C1
CC(C)(C)OC(=O)NCC1CNC1
null
[OH-].[OH-].[Pd+2]
CO
Deprotection
Hydrogenolysis of tertiary amines
b1d315bef48d6a81e10fb4eab17bea03d13eb9363139421badf3e724cd9c125a
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
C1CNC1
[C:1]1-[C:2]-[N;H0;D3;+0:3](-C(-c2:c:c:c:c:c:2)-c2:c:c:c:c:c:2)-[C:4]-1>>[C:1]1-[C:2]-[NH;D2;+0:3]-[C:4]-1
67.1
[{"value": 67.0, "product": "C(C)(C)(C)OC(=O)NCC1CNC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 67.1, "product": "C(C)(C)(C)OC(=O)NCC1CNC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
3.4 g (9.6 mmol) of 3-(N-tert-butyloxycarbonylaminomethyl)-1-benzhydryl azetidine was dissolved in 170 mL MeOH and hydrogenated over 0.30 g Pd(OH)2 at 5 MPa over night. The catalyst was filtered off and the solvent evaporated. The crude product was purified by flash chromatography using MeOH/CH2Cl2, 1/9, followed by Me...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.c1ccccc1.C1C[NH]C1
C1CNC1
C1CNC1
Other
[OH-].[OH-].[Pd+2].CO
null
null
CC(C)(C)OC(=O)NCC1CN(C(c2ccccc2)c2ccccc2)C1>[OH-].[OH-].[Pd+2].CO>CC(C)(C)OC(=O)NCC1CNC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6d13e77736d347fc8d7ecd3394515558
CC(C)(C)OC(=O)NCC1CNC1.COC(=N)NC(=O)OCc1ccccc1>>CC(C)(C)OC(=O)NCC1CN(C(=N)NC(=O)OCc2ccccc2)C1
C(C)(C)(C)OC(=O)NCC1CNC1.C(C1=CC=CC=C1)OC(=O)NC(OC)=N>>C(C)(C)(C)OC(=O)NCC1CN(C1)C(NC(=O)OCC1=CC=CC=C1)=N
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH:10]1[CH2:11][NH:12][CH2:26]1.CO[C:13](=[NH:14])[NH:15][C:16](=[O:17])[O:18][CH2:19][c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH:10]1[CH2:11][N:12]([C:13](=[NH:14])[NH:15][C:16](=[O:17])[O:18...
CC(C)(C)OC(=O)NCC1CNC1.COC(=N)NC(=O)OCc1ccccc1
CC(C)(C)OC(=O)NCC1CN(C(=N)NC(=O)OCc2ccccc2)C1
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
df9d7c4a76f1544cef1093b3238ae3b2a5398bdd8f2dfa35c3397eb37c957b67
f41a0ac1ece338534be38b696cb3541e6003cebbbc2e76e91361a568e6946ab0
N=C(NC(=O)OCc1ccccc1)N1CCC1
C-O-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[C:4](-[#8:5])=[O;D1;H0:6].[C:7]1-[C:8]-[NH;D2;+0:9]-[C:10]-1>>[#8:5]-[C:4](=[O;D1;H0:6])-[#7:3]-[C;H0;D3;+0:1](=[N;D1;H1:2])-[N;H0;D3;+0:9]1-[C:8]-[C:7]-[C:10]-1
38.5
[{"value": 38.0, "product": "C(C)(C)(C)OC(=O)NCC1CN(C1)C(NC(=O)OCC1=CC=CC=C1)=N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 38.5, "product": "C(C)(C)(C)OC(=O)NCC1CN(C1)C(NC(=O)OCC1=CC=CC=C1)=N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
72
HOUR
0.9 g (4.8 mmol) of 3-(N-tert-butyloxycarbonylaminomethyl) azetidine and 1.3 g (6.3 mmol) of N-benzyloxycarbonyl-O-methylisourea was mixed in 6.5 mL toluene and heated to 70° C. for 72 h and then left at room temperature for another 72 h. Evaporation followed by flash chromatography using EtOAc followed by MeOH (satura...
10.6084/m9.figshare.5104873.v1
null
Ether.Secondary amine
Tertiary amine
C1CNC1
C1C[NH]C1
C1C[NH]C1.c1ccccc1
HO-
C1(=CC=CC=C1)C
70
72
CC(C)(C)OC(=O)NCC1CNC1.COC(=N)NC(=O)OCc1ccccc1>C1(=CC=CC=C1)C>CC(C)(C)OC(=O)NCC1CN(C(=N)NC(=O)OCc2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-df1a0a7ecbb7442b9ee9a9bf29ebf6f4
N#CCC1CN(C(c2ccccc2)c2ccccc2)C1>>NCCC1CN(C(c2ccccc2)c2ccccc2)C1
C(#N)CC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[H-]>>NCCC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1
[N:1]#[C:2][CH2:3][CH:4]1[CH2:5][N:6]([CH:7]([c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[c:14]2[cH:15][cH:16][cH:17][cH:18][cH:19]2)[CH2:20]1>>[NH2:1][CH2:2][CH2:3][CH:4]1[CH2:5][N:6]([CH:7]([c:8]2[cH:9][cH:10][cH:11][cH:12][cH:13]2)[c:14]2[cH:15][cH:16][cH:17][cH:18][cH:19]2)[CH2:20]1
N#CCC1CN(C(c2ccccc2)c2ccccc2)C1
NCCC1CN(C(c2ccccc2)c2ccccc2)C1
null
null
C1CCOC1
Reduction
Reduction of nitrile to amine
65bec2d9f430701d30dc9fcbe1c5418f3dfa174d67be035c50edfc71895dc9c7
e8d1bc928b94bd4f5bf4b23363ce8f88b1ce7d146ba93829e7b8ad8dbe0007a7
c1ccc(C(c2ccccc2)N2CCC2)cc1
[C:1]-[C:2]-[C;H0;D2;+0:3]#[N;H0;D1;+0:4]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[NH2;D1;+0:4]
87
[{"value": 87.0, "product": "NCCC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.5, "product": "NCCC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
5.7 g (21.7 mmol) of 3-cyanomethyl-1-benzhydryl azetidine was added slowly to a suspension of 2.9 g (76.0 mmol) of LiAlH4 in 80 mL of dry THF at roomtemperature. The reaction mixture was refluxed for 4 h. Excess hydride reagent was hydrolyzed by careful addition, with cooling, of NH4 Cl(aq), the gelatinous mixture was ...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
C1C[NH]C1.c1ccccc1.c1ccccc1
null
C1CCOC1
null
null
N#CCC1CN(C(c2ccccc2)c2ccccc2)C1>C1CCOC1>NCCC1CN(C(c2ccccc2)c2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f30681c7d0b3464187d3580e892ca811
CC(C)(C)OC(=O)NCC1CN(C(c2ccccc2)c2ccccc2)C1.NCCC1CN(C(c2ccccc2)c2ccccc2)C1>>CC(C)(C)OC(=O)NCCC1CN(C(c2ccccc2)c2ccccc2)C1
NCCC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1.C(C)(C)(C)OC(=O)NCC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1>>C(C)(C)(C)OC(=O)NCCC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1
c1ccc(C(c2ccccc2)N2CC([CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])C2)cc1.NC[CH2:10][CH:11]1[CH2:12][N:13]([CH:14]([c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[c:21]2[cH:22][cH:23][cH:24][cH:25][cH:26]2)[CH2:27]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH:11]1[CH2:12][N:1...
CC(C)(C)OC(=O)NCC1CN(C(c2ccccc2)c2ccccc2)C1.NCCC1CN(C(c2ccccc2)c2ccccc2)C1
CC(C)(C)OC(=O)NCCC1CN(C(c2ccccc2)c2ccccc2)C1
null
null
null
C-C Coupling
Boc amine protection of primary amine
d521418afe2b27744aa0853d3dbd8c645ea76c2c7dd653b84e848b47bf48524a
add7b52e4edbeac1e43fd32b2de1efd36d163c3f3297283b5665fda49bd05248
c1ccc(C(c2ccccc2)N2CCC2)cc1
N-C-[CH2;D2;+0:1]-[C:2]1-[C:3]-[#7:4]-[C:5]-1.[C;D1;H3:6]-[C:7](-[C;D1;H3:8])(-[C;D1;H3:9])-[#8:10]-[C:11](=[O;D1;H0:12])-[#7:13]-[CH2;D2;+0:14]-C1-C-N(-C(-c2:c:c:c:c:c:2)-c2:c:c:c:c:c:2)-C-1>>[C;D1;H3:6]-[C:7](-[C;D1;H3:8])(-[C;D1;H3:9])-[#8:10]-[C:11](=[O;D1;H0:12])-[#7:13]-[CH2;D2;+0:14]-[CH2;D2;+0:1]-[C:2]1-[C:3]-[...
null
[]
null
null
null
null
The title compound was prepared from 3-aminoethyl-1-benzhydryl azetidine according the procedure for 3-(N-tert-butyloxycarbonylaminomethyl)-1-benzhydryl azetidine, in a yield of 6.5 g (95%). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amine.Tertiary amine
null
c1ccccc1.c1ccccc1.C1CNC1
null
C1C[NH]C1.c1ccccc1.c1ccccc1
Other
null
null
null
CC(C)(C)OC(=O)NCC1CN(C(c2ccccc2)c2ccccc2)C1.NCCC1CN(C(c2ccccc2)c2ccccc2)C1>>CC(C)(C)OC(=O)NCCC1CN(C(c2ccccc2)c2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-b116e8105ba1433db653190ba3814a43
CC(C)(C)OC(=O)NCCC1CN(C(c2ccccc2)c2ccccc2)C1>>CC(C)(C)OC(=O)NCCC1CNC1
C(C)(C)(C)OC(=O)NCCC1CN(C1)C(C1=CC=CC=C1)C1=CC=CC=C1.C(C)(C)(C)OC(=O)NCC1CNC1>>C(C)(C)(C)OC(=O)NCCC1CNC1
c1ccc(C(c2ccccc2)[N:13]2[CH2:12][CH:11]([CH2:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:14]2)cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH:11]1[CH2:12][NH:13][CH2:14]1
CC(C)(C)OC(=O)NCCC1CN(C(c2ccccc2)c2ccccc2)C1
CC(C)(C)OC(=O)NCCC1CNC1
null
null
null
Deprotection
Hydrogenolysis of tertiary amines
b1d315bef48d6a81e10fb4eab17bea03d13eb9363139421badf3e724cd9c125a
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
C1CNC1
[C:1]1-[C:2]-[N;H0;D3;+0:3](-C(-c2:c:c:c:c:c:2)-c2:c:c:c:c:c:2)-[C:4]-1>>[C:1]1-[C:2]-[NH;D2;+0:3]-[C:4]-1
null
[]
null
null
null
null
The title compound was prepared from 3-(N-tert-butyloxycarbonylaminoethyl)-1-benzhydryl azetidine according the procedure for 3-(N-tert-butyloxycarbonylaminomethyl) azetidine, in a yield of 1.2 g (70%). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.c1ccccc1.C1C[NH]C1
C1CNC1
C1CNC1
Other
null
null
null
CC(C)(C)OC(=O)NCCC1CN(C(c2ccccc2)c2ccccc2)C1>>CC(C)(C)OC(=O)NCCC1CNC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8f3a40523b2f4c598bcdee0f2ca4642e
CC(C)(C)OC(=O)NCC1CN(C(=N)NC(=O)OCc2ccccc2)C1.CC(C)(C)OC(=O)NCCC1CNC1>>CC(C)(C)OC(=O)NCCC1CN(C(=N)NC(=O)OCc2ccccc2)C1
C(C)(C)(C)OC(=O)NCCC1CNC1.C(C)(C)(C)OC(=O)NCC1CN(C1)C(NC(=O)OCC1=CC=CC=C1)=N>>C(C)(C)(C)OC(=O)NCCC1CN(C1)C(NC(=O)OCC1=CC=CC=C1)=N
CC(C)(C)OC(=O)N[CH2:10][CH:11]1[CH2:12][N:13]([C:14](=[NH:15])[NH: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.C1NCC1C[CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH:11]1[CH2:12][N:13]([C:14]...
CC(C)(C)OC(=O)NCC1CN(C(=N)NC(=O)OCc2ccccc2)C1.CC(C)(C)OC(=O)NCCC1CNC1
CC(C)(C)OC(=O)NCCC1CN(C(=N)NC(=O)OCc2ccccc2)C1
null
null
null
C-C Coupling
OtherReaction
1d7ac5a0e7f04e0106eb9b0e5a3a46be2ebfbf5433f9d9401383a34517b64867
6ace98d3c3046eaaa61eca3c25430e6bc592d0da17160c18a7110f07cdb4d09d
N=C(NC(=O)OCc1ccccc1)N1CCC1
C-C(-C)(-C)-O-C(=O)-N-[CH2;D2;+0:1]-[C:2]1-[C:3]-[#7:4]-[C:5]-1.[C;D1;H3:6]-[C:7](-[C;D1;H3:8])(-[C;D1;H3:9])-[#8:10]-[C:11](=[O;D1;H0:12])-[#7:13]-[CH2;D2;+0:14]-C-C1-C-N-C-1>>[C;D1;H3:6]-[C:7](-[C;D1;H3:8])(-[C;D1;H3:9])-[#8:10]-[C:11](=[O;D1;H0:12])-[#7:13]-[CH2;D2;+0:14]-[CH2;D2;+0:1]-[C:2]1-[C:3]-[#7:4]-[C:5]-1
null
[]
null
null
null
null
The title compound was prepared from 3-(N-tert-butyloxycarbonylaminoethyl) azetidine according the procedure for 3-(N-tert-butyloxycarbonylaminomethyl)-1-(N-benzyloxycarbon ylamidino) azetidine, in a yield of 0.090 g (34%). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Secondary amine.Boc
null
C1CNC1
null
C1C[NH]C1.c1ccccc1
HO-
null
null
null
CC(C)(C)OC(=O)NCC1CN(C(=N)NC(=O)OCc2ccccc2)C1.CC(C)(C)OC(=O)NCCC1CNC1>>CC(C)(C)OC(=O)NCCC1CN(C(=N)NC(=O)OCc2ccccc2)C1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f2917c57d8924daa80ca9144336b9913
CSC[C@H](N)C(=O)O.O=[N+]([O-])c1ccc(F)cc1F>>CSC[C@H](Nc1cc(F)ccc1[N+](=O)[O-])C(=O)O
CSC[C@H](N)C(=O)O.C(C)N(CC)CC.FC1=C(C=CC(=C1)F)[N+](=O)[O-]>>FC=1C=CC(=C(C1)N[C@@H](CSC)C(=O)O)[N+](=O)[O-]
[CH3:1][S:2][CH2:3][C@H:4]([NH2:5])[C:16](=[O:17])[OH:18].F[c:6]1[cH:7][c:8]([F:9])[cH:10][cH:11][c:12]1[N+:13](=[O:14])[O-:15]>>[CH3:1][S:2][CH2:3][C@H:4]([NH:5][c:6]1[cH:7][c:8]([F:9])[cH:10][cH:11][c:12]1[N+:13](=[O:14])[O-:15])[C:16](=[O:17])[OH:18]
CSC[C@H](N)C(=O)O.O=[N+]([O-])c1ccc(F)cc1F
CSC[C@H](Nc1cc(F)ccc1[N+](=O)[O-])C(=O)O
null
null
O.CC(=O)C
Heteroatom Alkylation and Arylation
Buchwald-Hartwig/Ullmann-Goldberg/N-arylation primary amine
da9dae6a655c4bd18887b692f91621e77027436294d6e1fc7be7295afb364796
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#7;+:5]):[c:6].[C:7]-[C:8](-[NH2;D1;+0:9])-[C:10](=[O;D1;H0:11])-[O;D1;H1:12]>>[#7;+:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[NH;D2;+0:9]-[C:8](-[C:7])-[C:10](=[O;D1;H0:11])-[O;D1;H1:12]):[c:2]:[c:3]
null
[]
null
null
null
null
16.2 g of (-)-S-Methyl-L-cysteine (0.1 mol) are suspended in a mixture of 120 ml of water and 120 ml of acetone in a four-necked flask under N2. 30.4 ml (22.2 g) of triethylamine (0.22 mol) are added rapidly while stirring. 15.9 g of 2,4-difluoronitrobenzene (0.1 mol) are added, with further stirring, to the resulting ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccccc1
c1ccccc1
c1ccccc1
HF
O.CC(=O)C
null
null
CSC[C@H](N)C(=O)O.O=[N+]([O-])c1ccc(F)cc1F>O.CC(=O)C>CSC[C@H](Nc1cc(F)ccc1[N+](=O)[O-])C(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-49f2d19dd08c44a6a1032e78dc4359e1
CSC[C@H](Nc1cc(F)ccc1[N+](=O)[O-])C(=O)O.C[O-]>>COc1ccc([N+](=O)[O-])c(N[C@@H](CSC)C(=O)O)c1
FC=1C=CC(=C(C1)N[C@@H](CSC)C(=O)O)[N+](=O)[O-].C[O-].[Na+]>>COC=1C=CC(=C(C1)N[C@@H](CSC)C(=O)O)[N+](=O)[O-]
F[c:3]1[cH:4][cH:5][c:6]([N+:7](=[O:8])[O-:9])[c:10]([NH:11][C@@H:12]([CH2:13][S:14][CH3:15])[C:16](=[O:17])[OH:18])[cH:19]1.[CH3:1][O-:2]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([N+:7](=[O:8])[O-:9])[c:10]([NH:11][C@@H:12]([CH2:13][S:14][CH3:15])[C:16](=[O:17])[OH:18])[cH:19]1
CSC[C@H](Nc1cc(F)ccc1[N+](=O)[O-])C(=O)O.C[O-]
COc1ccc([N+](=O)[O-])c(N[C@@H](CSC)C(=O)O)c1
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
39d5ff1cd4e8c0faf94cc5b2ad4bb50293cf15e9a5e1331d02f5731b7900363c
51fd03eb6a688046e417b9ed09ea0e72062396d005af1318b9b5f376a97da959
c1ccccc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[C;D1;H3:6]-[O-;H0;D1:7]>>[C;D1;H3:6]-[O;H0;D2;+0:7]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
null
null
27 g of N-(5-fluoro-2-nitrophenyl)-S-methyl-L-cysteine (0.1 mol) from Example 1 are dissolved in 150 ml of absolute methanol in a four-necked flask, and 14.4 g of 95% sodium methoxide (0.25 mmol) are added in portions, within the space of 20 minutes and under argon, to this solution while stirring well and while coolin...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Ether
c1ccccc1
c1ccccc1
c1ccccc1
Other
CO
null
null
CSC[C@H](Nc1cc(F)ccc1[N+](=O)[O-])C(=O)O.C[O-]>CO>COc1ccc([N+](=O)[O-])c(N[C@@H](CSC)C(=O)O)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-acafbcbe9a2a44309d2b4dd92b3f58bb
OCCCCc1ccccc1>>O=CCCCc1ccccc1
C1(=CC=CC=C1)CCCCO.[Cr](=O)(=O)([O-])Cl.C=1C=C[NH+]=CC1.[O-][Cr](=O)(=O)Cl>>C1(=CC=CC=C1)CCCC=O
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1>>[O:1]=[CH:2][CH2:3][CH2:4][CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1
OCCCCc1ccccc1
O=CCCCc1ccccc1
null
null
CCOCC.C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccccc1
[C:1]-[C:2]-[CH2;D2;+0:3]-[OH;D1;+0:4]>>[C:1]-[C:2]-[CH;D2;+0:3]=[O;H0;D1;+0:4]
22.7
[{"value": 22.7, "product": "C1(=CC=CC=C1)CCCC=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
To a solution of 3.2 mL (20.8 mmol) of 4-phenyl-1-butanol (Aldrich Chemical Co.) in 20 mL of CH2Cl2 at 0° C. was added 3.2 g of powdered 3 Å molecular sieves and then 5.37 g (24.9 mmol) of pyridinum chlorochromate (PCC). The resulting suspension was stirred at 0° C. for 1 h at which time an additional 2.16 g (10.0 mmol...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccccc1
null
CCOCC.C(Cl)Cl
null
0.5
OCCCCc1ccccc1>CCOCC.C(Cl)Cl>O=CCCCc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-76f829bb3ada43dbb9e69131f368da79
O=CCCCc1ccccc1.[Br][Mg][CH2]CCc1ccccc1>>OC(CCCc1ccccc1)CCCc1ccccc1
C1(=CC=CC=C1)CCCC=O.C1(=CC=CC=C1)CCC[Mg]Br>>C1(=CC=CC=C1)CCCC(CCCC1=CC=CC=C1)O
[O:1]=[CH:2][CH2:12][CH2:13][CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1.[Br][Mg][CH2:3][CH2:4][CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1>>[OH:1][CH:2]([CH2:3][CH2:4][CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1)[CH2:12][CH2:13][CH2:14][c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1
O=CCCCc1ccccc1.[Br][Mg][CH2]CCc1ccccc1
OC(CCCc1ccccc1)CCCc1ccccc1
null
null
C1CCOC1
C-C Coupling
Grignard from aldehyde to alcohol
fec51c6fbcca146daa523566f7e8d93ddaee19549cd7ca45d0ef939f0a2ea2fd
38fa131ecaada942f85a297b49034b58ccef3f2e8ba6de5e28a59b5f4292ff1f
c1ccc(CCCCCCCc2ccccc2)cc1
[Br]-[Mg]-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[C:5]-[CH;D2;+0:6]=[O;H0;D1;+0:7]>>[C:4]-[C:5]-[CH;D3;+0:6](-[OH;D1;+0:7])-[CH2;D2;+0:1]-[C:2]-[C:3]
88.8
[{"value": 88.8, "product": "C1(=CC=CC=C1)CCCC(CCCC1=CC=CC=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
0.5
HOUR
To a solution of 700 mg (4.7 mmol) of 4-phenyl-1-butanal (119) in 5.0 mL of THF at 0° C. was added 10.0 mL (5.0 mmol) of 3-phenyl-1-propylmagnesium bromide (120) and the resulting mixture was stirred at 0° C. for 0.5 h. The mixture was then quenched by the dropwise addition of saturated NH4Cl and diluted with ether. Th...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Aldehyde
Secondary alcohol
null
null
c1ccccc1.c1ccccc1
Br-.Mg
C1CCOC1
0
0.5
O=CCCCc1ccccc1.[Br][Mg][CH2]CCc1ccccc1>C1CCOC1>OC(CCCc1ccccc1)CCCc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1489d72d83a3432b8980d4f94eed3de6
OCc1cccc(Oc2ccccc2)c1>>O=Cc1cccc(Oc2ccccc2)c1
O(C1=CC=CC=C1)C=1C=C(CO)C=CC1>>O(C1=CC=CC=C1)C=1C=C(C=O)C=CC1
[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][c:7]([O:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[cH:15]1>>[O:1]=[CH:2][c:3]1[cH:4][cH:5][cH:6][c:7]([O:8][c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[cH:15]1
OCc1cccc(Oc2ccccc2)c1
O=Cc1cccc(Oc2ccccc2)c1
null
O=[Mn]=O.O=[Mn]=O
C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccc(Oc2ccccc2)cc1
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]
90.1
[{"value": 90.1, "product": "O(C1=CC=CC=C1)C=1C=C(C=O)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
To a solution of 1.8mL (10.3 mmol) of 3-phenoxybenzyl alcohol (Aldrich Chemical Co.) in 20 mL of CH2Cl2 at room temperature was added 1.5 g of powdered 4 Å molecular sieves and 2.5 g of activated MnO2. The resulting suspension was stirred at room temperature for 0.5 h, at which time an additional 2.5 g of MnO2 was adde...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccccc1.c1ccccc1
null
O=[Mn]=O.O=[Mn]=O.C(Cl)Cl
null
0.5
OCc1cccc(Oc2ccccc2)c1>O=[Mn]=O.O=[Mn]=O.C(Cl)Cl>O=Cc1cccc(Oc2ccccc2)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2a5760aaa3d049789dc0038907f707bb
C/C(=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1)CO>>C/C(C=O)=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1
C(C)N(CC)CC.[Si](C)(C)(C(C)(C)C)O[C@@H]1CC[C@H](CC1)/C=C(/CO)\C.C(C(=O)Cl)(=O)Cl.CS(=O)C>>[Si](C)(C)(C(C)(C)C)O[C@@H]1CC[C@H](CC1)/C=C(/C=O)\C
[CH3:1]/[C:2]([CH2:3][OH:4])=[CH:5]\[C@H:6]1[CH2:7][CH2:8][C@H:9]([O:10][Si:11]([CH3:12])([CH3:13])[C:14]([CH3:15])([CH3:16])[CH3:17])[CH2:18][CH2:19]1>>[CH3:1]/[C:2]([CH:3]=[O:4])=[CH:5]\[C@H:6]1[CH2:7][CH2:8][C@H:9]([O:10][Si:11]([CH3:12])([CH3:13])[C:14]([CH3:15])([CH3:16])[CH3:17])[CH2:18][CH2:19]1
C/C(=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1)CO
C/C(C=O)=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1
null
null
C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
C1CCCCC1
[C:1]-[C:2](/[C:3]=[C:4](\[C;D1;H3:5])-[CH2;D2;+0:6]-[OH;D1;+0:7])-[C:8]>>[C:1]-[C:2](/[C:3]=[C:4](\[C;D1;H3:5])-[CH;D2;+0:6]=[O;H0;D1;+0:7])-[C:8]
null
[]
null
null
5
MINUTE
To a -78° C. solution of oxalyl chloride (105 μL, 1.2 mmol) in 1.0 mL of methylene chloride was added dimethylsulfoxide (170 μL, 2.4 mmol). The resulting solution was stirred for 5 min and then 170 mg (0.6 mmol) of the alcohol 135 was added in 1.0 mL of methylene chloride. The reaction mixture was stirred at -78° C. fo...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
C1CCCCC1
null
C(Cl)Cl
null
0.083333
C/C(=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1)CO>C(Cl)Cl>C/C(C=O)=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a6be5895ebf2488a874923e3878acfbe
C/C(C=O)=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1.OC(CCCc1ccccc1)CCCc1ccccc1>>C/C(=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1)C(O)CCCc1ccccc1
[Si](C)(C)(C(C)(C)C)O[C@@H]1CC[C@H](CC1)/C=C(/C=O)\C.C1(=CC=CC=C1)CCC[Mg]Br.C1(=CC=CC=C1)CCCC(CCCC1=CC=CC=C1)O>>[Si](C)(C)(C(C)(C)C)O[C@@H]1CC[C@H](CC1)\C=C(\C(CCCC1=CC=CC=C1)O)/C
[CH3:1]/[C:2](=[CH:3]\[C@H:4]1[CH2:5][CH2:6][C@H:7]([O:8][Si:9]([CH3:10])([CH3:11])[C:12]([CH3:13])([CH3:14])[CH3:15])[CH2:16][CH2:17]1)[CH:18]=[O:19].OC(CCCc1ccccc1)[CH2:20][CH2:21][CH2:22][c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[CH3:1]/[C:2](=[CH:3]\[C@H:4]1[CH2:5][CH2:6][C@H:7]([O:8][Si:9]([CH3:10])([CH3:11])[C...
C/C(C=O)=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1.OC(CCCc1ccccc1)CCCc1ccccc1
C/C(=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1)C(O)CCCc1ccccc1
null
null
C1CCOC1
C-C Coupling
OtherReaction
745e9d5550f1bc5d8f9663a93679046bd7d0fca4f985bc640e2b19519b4d19c5
a3560394ead03d025274020cb23d2d580daa991ec04104aa7a504d5ac71e3ae6
C(=CC1CCCCC1)CCCCc1ccccc1
O-C(-C-C-C-c1:c:c:c:c:c:1)-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[C:5](/[C:6]=[C:7](\[C;D1;H3:8])-[CH;D2;+0:9]=[O;H0;D1;+0:10])-[C:11]>>[C:4]-[C:5](/[C:6]=[C:7](\[C;D1;H3:8])-[CH;D3;+0:9](-[OH;D1;+0:10])-[CH2;D2;+0:1]-[C:2]-[C:3])-[C:11]
null
[]
null
null
null
null
The alcohol 137 was prepared from the crude aldehyde 136. and 1.5 mL (0.75 mmol) of 120 in 2.0 mL of THF as described above for the synthesis of alcohol 121 in Example 1 to give 220 mg of the crude diastereomeric alcohol 137. Flash chromatography (elution with 20% ethyl acetate in hexane) afforded 146 mg of the alcohol...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary alcohol
Secondary alcohol
c1ccccc1
null
C1CCCCC1.c1ccccc1
HO-
C1CCOC1
null
null
C/C(C=O)=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1.OC(CCCc1ccccc1)CCCc1ccccc1>C1CCOC1>C/C(=C\[C@@H]1CC[C@@H](O[Si](C)(C)C(C)(C)C)CC1)C(O)CCCc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5ab94114d8b645e082906ef9a74075cf
CN(C)O.O=C(O)CCCc1c[nH]c2ccccc12>>CON(C)C(=O)CCCc1c[nH]c2ccccc12
N1C=C(C2=CC=CC=C12)CCCC(=O)O.C(C)(C)N(C(C)C)CC.Cl.CN(O)C.F[P-](F)(F)(F)(F)F.N1(N=NC2=C1C=CC=C2)O[P+](N(C)C)(N(C)C)N(C)C>>CN(C(CCCC1=CNC2=CC=CC=C12)=O)OC
[CH3:1][N:3]([OH:2])[CH3:4].O[C:5](=[O:6])[CH2:7][CH2:8][CH2:9][c:10]1[cH:11][nH:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12>>[CH3:1][O:2][N:3]([CH3:4])[C:5](=[O:6])[CH2:7][CH2:8][CH2:9][c:10]1[cH:11][nH:12][c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12
CN(C)O.O=C(O)CCCc1c[nH]c2ccccc12
CON(C)C(=O)CCCc1c[nH]c2ccccc12
null
null
C(C)#N
Acylation
OtherReaction
d8b2983456520e04d3c60473cdb132720f2fe2d412f78ff14b19d4ff149b7970
24bc53ff5c10681d8cc73a1bb4d5e3f184958ea20e029afafa8ff123b17ea76c
c1ccc2[nH]ccc2c1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C;D1;H3:5]-[N;H0;D3;+0:6](-[CH3;D1;+0:7])-[OH;D1;+0:8]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:6](-[C;D1;H3:5])-[O;H0;D2;+0:8]-[CH3;D1;+0:7]
94.3
[{"value": 94.3, "product": "CN(C(CCCC1=CNC2=CC=CC=C12)=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a slurry of 1.75 g (8.61 mmol) of 3-indolebutyric acid (Aldrich Chemical Co.) in acetonitrile at room temperature was added 7.0 mL (40.2 mmol) of N,N-diisopropylethylamine, 1.0 g (10.3 mmol) of N,N-dimethylhydroxylamine hydrochloride and 4.19 g (9.5 mmol) of benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafl...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Tertiary amine
Tertiary amide
null
null
c1ccc2[nH]ccc2c1
HO-
C(C)#N
null
8
CN(C)O.O=C(O)CCCc1c[nH]c2ccccc12>C(C)#N>CON(C)C(=O)CCCc1c[nH]c2ccccc12
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-70019092bb2c48d18020b5be4b31c9ad
CON(C)C(=O)CCCc1c[nH]c2ccccc12.[Cl][Mg][CH2]c1ccccc1>>O=C(CCC(Cc1ccccc1)c1c[nH]c2ccccc12)CCC(Cc1ccccc1)c1c[nH]c2ccccc12
CN(C(CCCC1=CNC2=CC=CC=C12)=O)OC.C(C1=CC=CC=C1)[Mg]Cl>>C(C1=CC=CC=C1)C(CCC(=O)CCC(CC1=CC=CC=C1)C1=CNC2=CC=CC=C12)C1=CNC2=CC=CC=C12
O([CH3:3])[N:15]([C:2](=[O:1])[CH2:22][CH2:23][CH2:24][c:32]1[cH:33][nH:34][c:35]2[cH:36][cH:37][cH:38][cH:39][c:40]12)[CH3:14].[Cl][Mg][CH2:6][c:7]1[cH:8][cH:18][cH:19][cH:20][cH:21]1>>[O:1]=[C:2]([CH2:3][CH2:4][CH:5]([CH2:6][c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1)[c:13]1[cH:14][nH:15][c:16]2[cH:17][cH:18][cH:19][cH:...
CON(C)C(=O)CCCc1c[nH]c2ccccc12.[Cl][Mg][CH2]c1ccccc1
O=C(CCC(Cc1ccccc1)c1c[nH]c2ccccc12)CCC(Cc1ccccc1)c1c[nH]c2ccccc12
null
null
C1CCOC1
Aromatic Heterocycle Formation
OtherReaction
298d2d31c7f84c015c10da15c1d39cea10099f6fc8aa5162a1e949dce4f10daa
81f865b55a0aa641c7c58099315544d18d237b86f0e3509b1685b149b9ab86dc
O=C(CCC(Cc1ccccc1)c1c[nH]c2ccccc12)CCC(Cc1ccccc1)c1c[nH]c2ccccc12
[CH3;D1;+0:1]-[N;H0;D3;+0:2](-O-[CH3;D1;+0:3])-[C;H0;D3;+0:4](=[O;D1;H0:5])-[C:6]-[C:7]-[CH2;D2;+0:8]-[c:9]1:[c:10]:[#7;a:11]:[c:12]:[c:13]:1.[Cl]-[Mg]-[CH2;D2;+0:14]-[c;H0;D3;+0:15]1:[cH;D2;+0:16]:[c:17]:[c:18]:[cH;D2;+0:19]:[cH;D2;+0:20]:1>>[O;D1;H0:5]=[C;H0;D3;+0:4](-[C:6]-[C:7]-[CH;D3;+0:8](-[C:21]-[c:22])-[c:9]1:[...
68.6
[{"value": 68.6, "product": "C(C1=CC=CC=C1)C(CCC(=O)CCC(CC1=CC=CC=C1)C1=CNC2=CC=CC=C12)C1=CNC2=CC=CC=C12", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a solution of 147 mg (0.60 mmol) of amide 139 in 4.0 mL of THF at -78° C. was added 1.31 mL (1.31 mmol) of benzylmagnesium chloride (1.0M in Et2O) and the reaction mixture was allowed to warm to room temperature and stir for 3 h. The reaction was quenched with 5% KHSO4 and extracted into ether. The combined ethereal...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Tertiary amide
Ketone
c1ccccc1
c1ccccc1.c1ccc2[nH]ccc2c1.c1ccccc1
c1ccccc1.c1ccc2[nH]ccc2c1.c1ccccc1.c1ccc2[nH]ccc2c1
Mg
C1CCOC1
null
3
CON(C)C(=O)CCCc1c[nH]c2ccccc12.[Cl][Mg][CH2]c1ccccc1>C1CCOC1>O=C(CCC(Cc1ccccc1)c1c[nH]c2ccccc12)CCC(Cc1ccccc1)c1c[nH]c2ccccc12
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-741882d51dc940da96a4eb974652c9bb
O.O=Cc1ccccn1.[Li][CH2]CCC.c1ccc([P+](CCC2OCCCO2)(c2ccccc2)c2ccccc2)cc1>>C(=C/c1ccccn1)\CC1OCCCO1.C(=C\c1ccccn1)\CC1OCCCO1
N1=C(C=CC=C1)C=O.O.[Br-].O1C(OCCC1)CC[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.C(CCC)[Li]>>O1C(OCCC1)C/C=C/C1=NC=CC=C1.O1C(OCCC1)C\C=C/C1=NC=CC=C1
[OH2:26].[CH:2]([c:3]1[cH:4][cH:5][cH:6][cH:7][n:8]1)=[O:30].[Li][CH2:27][CH2:28][CH2:25][CH3:24].c1ccc([P+]([CH2:1][CH2:9][CH:10]2[O:11][CH2:12][CH2:13][CH2:14][O:15]2)([c:16]2ccc[cH:29]c2)[c:18]2[cH:17][cH:22][cH:21][cH:20][cH:19]2)cc1>>[CH:1](=[CH:2]/[c:3]1[cH:4][cH:5][cH:6][cH:7][n:8]1)\[CH2:9][CH:10]1[O:11][CH2:12...
O.O=Cc1ccccn1.[Li][CH2]CCC.c1ccc([P+](CCC2OCCCO2)(c2ccccc2)c2ccccc2)cc1
C(=C/c1ccccn1)\CC1OCCCO1.C(=C\c1ccccn1)\CC1OCCCO1
null
null
C1CCOC1
C-C Coupling
OtherReaction
7c66045ce7194fe655427ea5fa5c0dc6b626153f1009577225bfd7aa7dca8e9d
334880a3e534bf94c21ad10a2154b5e8216acf3dd3844c5e35907ff9e6afe03a
C(=C/c1ccccn1)\CC1OCCCO1.C(=C\c1ccccn1)\CC1OCCCO1
[#8:1]-[C:2](-[C:3]-[CH2;D2;+0:4]-[P+](-[c;H0;D3;+0:5]1:c:[cH;D2;+0:6]:c:c:c:1)(-[c;H0;D3;+0:7]1:[c:8]:[c:9]:[c:10]:[cH;D2;+0:11]:[cH;D2;+0:12]:1)-c1:c:c:c:c:c:1)-[#8:13].[CH3;D1;+0:14]-[CH2;D2;+0:15]-[CH2;D2;+0:16]-[CH2;D2;+0:17]-[Li].[O;H0;D1;+0:18]=[CH;D2;+0:19]-[c:20](:[c:21]):[#7;a:22]:[c:23].[OH2;D0;+0:24]>>[#7;a...
null
[]
0
CELSIUS
0.5
HOUR
To a suspension of 4.6 g (10.2 mmol) of [2-(1,3-dioxan-2yl)ethyl]triphenylphosphonium bromide (Aldrich Chemical Co.) in 50 mL of THF at 0° C. was added 6.4 mL (10.2 mmol) of n-butyl lithium (1.6M in hexanes) and the resulting red solution was allowed to stir at 0° C. for 0.5 h. To this solution was added 880 μL (9.3 mm...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Alkyl lithium
Ether.Ether
c1ccccc1.c1ccccc1.c1ccccc1
c1ccncc1.C1COCOC1
c1ccncc1.C1COCOC1.c1ccncc1.C1COCOC1
Li
C1CCOC1
0
0.5
O.O=Cc1ccccn1.[Li][CH2]CCC.c1ccc([P+](CCC2OCCCO2)(c2ccccc2)c2ccccc2)cc1>C1CCOC1>C(=C/c1ccccn1)\CC1OCCCO1.C(=C\c1ccccn1)\CC1OCCCO1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-600c0203d0174eabae949b47eb4ee810
C(=C\c1ccccn1)\CC1OCCCO1>>c1ccc(CCCC2OCCCO2)nc1
O1C(OCCC1)C\C=C/C1=NC=CC=C1>>O1C(OCCC1)CCCC1=NC=CC=C1
[cH:1]1[cH:2][cH:3][c:4](/[CH:5]=[CH:6]\[CH2:7][CH:8]2[O:9][CH2:10][CH2:11][CH2:12][O:13]2)[n:14][cH:15]1>>[cH:1]1[cH:2][cH:3][c:4]([CH2:5][CH2:6][CH2:7][CH:8]2[O:9][CH2:10][CH2:11][CH2:12][O:13]2)[n:14][cH:15]1
C(=C\c1ccccn1)\CC1OCCCO1
c1ccc(CCCC2OCCCO2)nc1
null
[Pd]
null
Reduction
Hydrogenation (double to single)
0bc3968b35f0839c230afb4215314da278abd4e1f10e42ec3012c5512de49ea5
312e9350dcad67590617294c0eb017edf0b9fbfe6133c06a3f393b871a889092
c1ccc(CCCC2OCCCO2)nc1
[#8:1]-[C:2](-[C:3]/[CH;D2;+0:4]=[CH;D2;+0:5]\[c:6](:[c:7]):[#7;a:8]:[c:9])-[#8:10]>>[#8:1]-[C:2](-[C:3]-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[c:6](:[c:7]):[#7;a:8]:[c:9])-[#8:10]
92.5
[{"value": 92.5, "product": "O1C(OCCC1)CCCC1=NC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Through a suspension of 800 mg (4.2 mmol) of olefin 149 and 100 mg of 10% palladium on carbon was bubbled a steady stream of hydrogen gas for a period of 10 min. The reaction mixture was then filtered through celite and concentrated to give 805 mg of the acetal 150 as a colorless oil. 1H NMR consistent with structure. ...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccncc1.C1COCOC1
null
[Pd]
null
null
C(=C\c1ccccn1)\CC1OCCCO1>[Pd]>c1ccc(CCCC2OCCCO2)nc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-dec073da1f4d41b387cb25d85d14d5f1
C[Si](C)(C)C=[N+]=[N-].O=Cc1ccc(C(=O)O)cc1>>COC(=O)c1ccc(C=O)cc1
C(=O)(O)C1=CC=C(C=O)C=C1.C[Si](C)(C)C=[N+]=[N-].C(=O)(O)[O-].[Na+]>>COC(C1=CC=C(C=C1)C=O)=O
C[Si](C)(C)[CH:1]=[N+]=[N-].[OH:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH:9]=[O:10])[cH:11][cH:12]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH:9]=[O:10])[cH:11][cH:12]1
C[Si](C)(C)C=[N+]=[N-].O=Cc1ccc(C(=O)O)cc1
COC(=O)c1ccc(C=O)cc1
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
O-alkylation of carboxylic acids with diazo compounds
39589be0e9a30df66714fe618d22a8ac0fb24901dbf2ead1ab33e31556c7ac64
8b539baf7aeb5ab868833e33306bad77200a853d562904197e13de2e27e229d7
c1ccccc1
C-[Si](-C)(-C)-[CH;D2;+0:1]=[N+]=[N-].[O;D1;H0:2]=[C:3](-[OH;D1;+0:4])-[c:5]>>[CH3;D1;+0:1]-[O;H0;D2;+0:4]-[C:3](=[O;D1;H0:2])-[c:5]
null
[]
0
CELSIUS
1
HOUR
To a suspension of 9.6 g (63.6 mmol) of 4-carboxybenzaldehyde (Aldrich Chemical Co.) in 100 mL of CH2Cl2 at 0° C. was added excess trimethylsilyldiazomethane and the resulting mixture was allowed to stir at 0° C. for 1 h. The mixture was poured into saturated aqueous NaHCO3 and extracted three times with ethyl acetate....
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Diazo.Silyl protective group
Ester
null
null
c1ccccc1
Other
C(Cl)Cl
0
1
C[Si](C)(C)C=[N+]=[N-].O=Cc1ccc(C(=O)O)cc1>C(Cl)Cl>COC(=O)c1ccc(C=O)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6120ae4e516c4335a3f2eb3671f18da1
CC(C1OCCCO1)[P+](c1ccccc1)(c1ccccc1)c1ccccc1.COC(=O)c1ccc(C=O)cc1>>COC(=O)c1ccc(C=CCC2OCCO2)cc1
COC(C1=CC=C(C=C1)C=O)=O.[Br-].O1C(OCCC1)C(C)[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.[Li]CCCC>>COC(C1=CC=C(C=C1)C=CCC1OCCO1)=O
c1ccc([P+](c2ccccc2)(c2ccccc2)[CH:11]([CH3:10])[CH:12]2[O:13]C[CH2:14][CH2:15][O:16]2)cc1.O=[CH:9][c:8]1[cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:18][cH:17]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]([CH:9]=[CH:10][CH2:11][CH:12]2[O:13][CH2:14][CH2:15][O:16]2)[cH:17][cH:18]1
CC(C1OCCCO1)[P+](c1ccccc1)(c1ccccc1)c1ccccc1.COC(=O)c1ccc(C=O)cc1
COC(=O)c1ccc(C=CCC2OCCO2)cc1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
e9b81df9c146ee18d35392a14925db0bee8ab8848c8cf94f2ebdbc4d1c5e0096
77f70c88f5781565bbef978a13aa26af9cfeac78f7ee0eea1b4ee8e9b7684280
C(=Cc1ccccc1)CC1OCCO1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[CH3;D1;+0:5]-[CH;D3;+0:6](-[C:7]1-[#8:8]-[C:9]-[CH2;D2;+0:10]-C-[O;H0;D2;+0:11]-1)-[P+](-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1>>[c:3]:[c:2](-[CH;D2;+0:1]=[CH;D2;+0:5]-[CH2;D2;+0:6]-[C:7]1-[#8:8]-[C:9]-[CH2;D2;+0:10]-[O;H0;D2;+0:11]-1):[c:4]
50.3
[{"value": 50.3, "product": "COC(C1=CC=C(C=C1)C=CCC1OCCO1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The olefin was prepared from 4.3 g (26.2 mmol) of the aldehyde 167, 13.94 g of [1-(1,3-dioxan-2-yl)ethyl]triphenylphosphoniumbromide and 12.6 mL (32.0 mmol) of n-BuLi in 75 mL of THF as described for the synthesis of 156 in Example 8. Flash chromatography (elution with 10% ethyl acetate in hexane) gave 3.27 g of the ol...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ether.Acetal/Ketal
Ether.Acetal/Ketal
c1ccccc1.c1ccccc1.c1ccccc1.C1COCOC1
C1COCO1
c1ccccc1.C1COCO1
HO-
C1CCOC1
null
null
CC(C1OCCCO1)[P+](c1ccccc1)(c1ccccc1)c1ccccc1.COC(=O)c1ccc(C=O)cc1>C1CCOC1>COC(=O)c1ccc(C=CCC2OCCO2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e4b7283463484f78b8ff3e4f5af4a115
COC(=O)c1ccc(CCCC2OCCO2)cc1>>OCc1ccc(CCCC2OCCCO2)cc1
COC(C1=CC=C(C=C1)CCCC1OCCO1)=O.[H-].C(C(C)C)[Al+]CC(C)C>>O1C(OCCC1)CCCC1=CC=C(C=C1)CO
O([C:2](=[O:1])[c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][CH2:9][CH:10]2[O:11][CH2:13][CH2:14][O:15]2)[cH:16][cH:17]1)[CH3:12]>>[OH:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][CH2:9][CH:10]2[O:11][CH2:12][CH2:13][CH2:14][O:15]2)[cH:16][cH:17]1
COC(=O)c1ccc(CCCC2OCCO2)cc1
OCc1ccc(CCCC2OCCCO2)cc1
null
null
C1CCOC1
Miscellaneous
OtherReaction
11ad31eb5e15c19b6b0bf870375e0b2b1b523d97d63cb564c0ec774ecdc4a360
60cbd0cdeedbe0df3b69ed77da0b18c75ba37a82153e9e68a6e5664d36d6e6bb
c1ccc(CCCC2OCCCO2)cc1
[CH3;D1;+0:1]-O-[C;H0;D3;+0:2](=[O;H0;D1;+0:3])-[c:4](:[c:5]):[c:6].[C:7]-[C:8]1-[#8:9]-[C:10]-[CH2;D2;+0:11]-[O;H0;D2;+0:12]-1>>[C:7]-[C:8]1-[#8:9]-[C:10]-[CH2;D2;+0:11]-[CH2;D2;+0:1]-[O;H0;D2;+0:12]-1.[OH;D1;+0:3]-[CH2;D2;+0:2]-[c:4](:[c:5]):[c:6]
95.8
[{"value": 95.8, "product": "O1C(OCCC1)CCCC1=CC=C(C=C1)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
15
MINUTE
To a solution of 2.85 g (11.4 mmol) of ester 169 in 25 mL of THF at 0° C. was added 4.4 mL (24.7 mmol) of diisobutylaluminum hydride and the resulting mixture was allowed to stir at 0° C. for 15 min. The reaction was quenched with saturated potassium sodium tartrate and extracted three times with ethyl acetate. The com...
10.6084/m9.figshare.5104873.v1
null
Ester.Ether
Ether.Primary alcohol.Acetal/Ketal
C1COCO1
C1COCOC1
c1ccccc1.C1COCOC1
Other
C1CCOC1
0
0.25
COC(=O)c1ccc(CCCC2OCCO2)cc1>C1CCOC1>OCc1ccc(CCCC2OCCCO2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2c93e9ea79a9405d9591cb8af2288670
CC(C)(C)[Si](Cl)(c1ccccc1)c1ccccc1.OCc1ccc(CCCC2OCCCO2)cc1>>CC(C)(C)[Si](OCc1ccc(CCCC2OCCO2)cc1)(c1ccccc1)c1ccccc1
O1C(OCCC1)CCCC1=CC=C(C=C1)CO.N1C=NC=C1.C(C)(C)(C)[Si](C1=CC=CC=C1)(C1=CC=CC=C1)Cl>>[Si](C1=CC=CC=C1)(C1=CC=CC=C1)(C(C)(C)C)OCC1=CC=C(C=C1)CCCC1OCCO1
Cl[Si:5]([C:2]([CH3:1])([CH3:3])[CH3:4])([c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1)[c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1.C1[O:16][CH:15]([CH2:14][CH2:13][CH2:12][c:11]2[cH:10][cH:9][c:8]([CH2:7][OH:6])[cH:21][cH:20]2)[O:19][CH2:18][CH2:17]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([O:6][CH2:7][c:8]1[cH:9][cH:10][c...
CC(C)(C)[Si](Cl)(c1ccccc1)c1ccccc1.OCc1ccc(CCCC2OCCCO2)cc1
CC(C)(C)[Si](OCc1ccc(CCCC2OCCO2)cc1)(c1ccccc1)c1ccccc1
null
null
C(Cl)Cl.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
9e413bc0d07ca62059d4b17c7c667341998c537dcec7980d48da74e43f2bda95
ac2b248fc44a91755024346efa1d4ec06dc3f9520fa06d3fd61d67db934b24ce
c1ccc([SiH](OCc2ccc(CCCC3OCCO3)cc2)c2ccccc2)cc1
Cl-[Si;H0;D4;+0:1](-[c:2](:[c:3]):[c:4])(-[c:5](:[c:6]):[c:7])-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:11].[C:12]-[C:13]1-[#8:14]-[C:15]-[CH2;D2;+0:16]-C-[O;H0;D2;+0:17]-1.[OH;D1;+0:18]-[C:19]-[c:20]>>[C;D1;H3:9]-[C:8](-[C;D1;H3:10])(-[C;D1;H3:11])-[Si;H0;D4;+0:1](-[O;H0;D2;+0:18]-[C:19]-[c:20])(-[c:2](:[c:3]):[c:4...
102.9
[{"value": 102.9, "product": "[Si](C1=CC=CC=C1)(C1=CC=CC=C1)(C(C)(C)C)OCC1=CC=C(C=C1)CCCC1OCCO1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 2.58 g (11.6 mmol) of alcohol 170 and 1.19 g (17.5 mmol) of imidazole in 50 mL of CH2Cl2 was added 3.4 mL (13.1 mmol) of tert-butylchlorodiphenyl silane and the resulting mixture was allowed to stir at room temperature for 1 h. The mixture was then diluted with ethyl acetate and washed with 0.5N HCl. T...
10.6084/m9.figshare.5104873.v1
null
Ether.Primary alcohol.Silyl protective group.Acetal/Ketal
Ether.Silyl protective group.Acetal/Ketal
C1COCOC1
C1COCO1
c1ccccc1.C1COCO1.c1ccccc1.c1ccccc1
HCl
C(Cl)Cl.C(C)(=O)OCC
null
1
CC(C)(C)[Si](Cl)(c1ccccc1)c1ccccc1.OCc1ccc(CCCC2OCCCO2)cc1>C(Cl)Cl.C(C)(=O)OCC>CC(C)(C)[Si](OCc1ccc(CCCC2OCCO2)cc1)(c1ccccc1)c1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-991308a13d764cc0817ac696051b408e
CC(C)(C)[Si](OCc1ccc(CCCC2OCCO2)cc1)(c1ccccc1)c1ccccc1>>CC(C)(C)[Si](OCc1ccc(CCCC=O)cc1)(c1ccccc1)c1ccccc1
Cl.[Si](C1=CC=CC=C1)(C1=CC=CC=C1)(C(C)(C)C)OCC1=CC=C(C=C1)CCCC1OCCO1.Cl.N1C=NC=C1.C(C)(C)(C)[Si](C1=CC=CC=C1)(C1=CC=CC=C1)Cl.C(=O)([O-])[O-].[K+].[K+]>>[Si](C1=CC=CC=C1)(C1=CC=CC=C1)(C(C)(C)C)OCC1=CC=C(C=C1)CCCC=O
C1C[O:16][CH:15]([CH2:14][CH2:13][CH2:12][c:11]2[cH:10][cH:9][c:8]([CH2:7][O:6][Si:5]([C:2]([CH3:1])([CH3:3])[CH3:4])([c:19]3[cH:20][cH:21][cH:22][cH:23][cH:24]3)[c:25]3[cH:26][cH:27][cH:28][cH:29][cH:30]3)[cH:18][cH:17]2)O1>>[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([O:6][CH2:7][c:8]1[cH:9][cH:10][c:11]([CH2:12][CH2:13][CH...
CC(C)(C)[Si](OCc1ccc(CCCC2OCCO2)cc1)(c1ccccc1)c1ccccc1
CC(C)(C)[Si](OCc1ccc(CCCC=O)cc1)(c1ccccc1)c1ccccc1
null
null
C1CCOC1
Miscellaneous
Acetal hydrolysis to aldehyde
f12636b09f9df336ccc8fe82b927db0e267bccc7cae0970f1f91c7ceed085225
84d5a69453aa750f462aa94a6bf2116fc17c5d88a9619aaa9eefb74b0c09848d
c1ccc(CO[SiH](c2ccccc2)c2ccccc2)cc1
[C:1]-[C:2]-[CH;D3;+0:3]1-O-C-C-[O;H0;D2;+0:4]-1>>[C:1]-[C:2]-[CH;D2;+0:3]=[O;H0;D1;+0:4]
42.8
[{"value": 42.8, "product": "[Si](C1=CC=CC=C1)(C1=CC=CC=C1)(C(C)(C)C)OCC1=CC=C(C=C1)CCCC=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 5.5 g (11.9 mmol) of the dioxolane 171 in 40 mL of THF at room temperature was added 40 mL of 4.0N HCl and the resulting solution was allowed to stir for 1 h. The mixture was neutralized with solid K2CO3, extracted with ethyl acetate and concentrated. The crude mixture was dissolved into 25 mL of CH2Cl...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Aldehyde
C1COCO1
null
c1ccccc1.c1ccccc1.c1ccccc1
HO-
C1CCOC1
null
1
CC(C)(C)[Si](OCc1ccc(CCCC2OCCO2)cc1)(c1ccccc1)c1ccccc1>C1CCOC1>CC(C)(C)[Si](OCc1ccc(CCCC=O)cc1)(c1ccccc1)c1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-796ad571c9a54fe982b77146ea41a2af
CC(C)(C)[Si](OCc1ccc(CCCC=O)cc1)(c1ccccc1)c1ccccc1.OC(CCCc1ccccc1)CCCc1ccccc1>>CC(C)(C)[Si](OCc1ccc(CCCC(O)CCCc2ccccc2)cc1)(c1ccccc1)c1ccccc1
[Si](C1=CC=CC=C1)(C1=CC=CC=C1)(C(C)(C)C)OCC1=CC=C(C=C1)CCCC=O.C1(=CC=CC=C1)CCC[Mg]Br.C1(=CC=CC=C1)CCCC(CCCC1=CC=CC=C1)O>>[Si](C1=CC=CC=C1)(C1=CC=CC=C1)(C(C)(C)C)OCC1=CC=C(C=C1)CCCC(CCCC1=CC=CC=C1)O
[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([O:6][CH2:7][c:8]1[cH:9][cH:10][c:11]([CH2:12][CH2:13][CH2:14][CH:15]=[O:16])[cH:26][cH:27]1)([c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1)[c:34]1[cH:35][cH:36][cH:37][cH:38][cH:39]1.OC(CCCc1ccccc1)[CH2:17][CH2:18][CH2:19][c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1>>[CH3:1][C:2]([CH3...
CC(C)(C)[Si](OCc1ccc(CCCC=O)cc1)(c1ccccc1)c1ccccc1.OC(CCCc1ccccc1)CCCc1ccccc1
CC(C)(C)[Si](OCc1ccc(CCCC(O)CCCc2ccccc2)cc1)(c1ccccc1)c1ccccc1
null
null
C1CCOC1
C-C Coupling
OtherReaction
745e9d5550f1bc5d8f9663a93679046bd7d0fca4f985bc640e2b19519b4d19c5
a3560394ead03d025274020cb23d2d580daa991ec04104aa7a504d5ac71e3ae6
c1ccc(CCCCCCCc2ccc(CO[SiH](c3ccccc3)c3ccccc3)cc2)cc1
O-C(-C-C-C-c1:c:c:c:c:c:1)-[CH2;D2;+0:1]-[C:2]-[C:3].[C:4]-[C:5]-[CH;D2;+0:6]=[O;H0;D1;+0:7]>>[C:4]-[C:5]-[CH;D3;+0:6](-[OH;D1;+0:7])-[CH2;D2;+0:1]-[C:2]-[C:3]
122.9
[{"value": 122.9, "product": "[Si](C1=CC=CC=C1)(C1=CC=CC=C1)(C(C)(C)C)OCC1=CC=C(C=C1)CCCC(CCCC1=CC=CC=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The alcohol 173 was prepared from 2.12 g (5.0 mmol) of 172 and 9.0 mL (9 mmol) of 120 in 50 mL of THF as described for the synthesis of 121 in Example 1. Flash chromatography (elution with 10% ethyl acetate in hexane) gave 3.3 g of the alcohol 173. 1H NMR consistent with the product. Conditions: See reaction.notes.proc...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary alcohol
Secondary alcohol
c1ccccc1
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HO-
C1CCOC1
null
null
CC(C)(C)[Si](OCc1ccc(CCCC=O)cc1)(c1ccccc1)c1ccccc1.OC(CCCc1ccccc1)CCCc1ccccc1>C1CCOC1>CC(C)(C)[Si](OCc1ccc(CCCC(O)CCCc2ccccc2)cc1)(c1ccccc1)c1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-696b27b131f24c17a8f31b09f5726b28
C[C@H](CO)Nc1ccccn1.O=S(Cl)Cl>>CC1CO[S@@](=O)N1c1ccccn1
N1=C(C=CC=C1)N[C@@H](CO)C.C(C)(C)N(C(C)C)CC.S(=O)(Cl)Cl>>CC1N([S@@](OC1)=O)C1=NC=CC=C1
[CH3:1][C@H:2]([CH2:3][OH:4])[NH:7][c:8]1[cH:9][cH:10][cH:11][cH:12][n:13]1.Cl[S:5](Cl)=[O:6]>>[CH3:1][CH:2]1[CH2:3][O:4][S@@:5](=[O:6])[N:7]1[c:8]1[cH:9][cH:10][cH:11][cH:12][n:13]1
C[C@H](CO)Nc1ccccn1.O=S(Cl)Cl
CC1CO[S@@](=O)N1c1ccccn1
null
null
ClCCl
Acylation
OtherReaction
3d2c53a666fb5a577b1313e56f6be1ee5645334dca79c4f10831a331b18034d8
b742aca93543b8e281f953dd08553590c1a12f1562393e6d8aed2fc78e477c3c
O=[S@@]1OCCN1c1ccccn1
Cl-[S;H0;D3;+0:1](-Cl)=[O;D1;H0:2].[C;D1;H3:3]-[C@H;D3;+0:4](-[C:5]-[OH;D1;+0:6])-[NH;D2;+0:7]-[c:8](:[c:9]):[#7;a:10]:[c:11]>>[C;D1;H3:3]-[CH;D3;+0:4]1-[C:5]-[O;H0;D2;+0:6]-[S@@;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:7]-1-[c:8](:[c:9]):[#7;a:10]:[c:11]
599.1
[{"value": 599.1, "product": "CC1N([S@@](OC1)=O)C1=NC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
A solution of (R)-N-(2-pyridyl)-2-aminopropanol (20.0 g, 0.13 moles) and N,N-diisopropylethylamine (33.6 g, 0.13 moles) in dichloromethane (500 ml) was cooled to 5° C. Then thionyl chloride (15.5 g, 0.13 moles) in dichloromethane (100 ml) was added slowly whilst the temperature was kept below 10° C. The mixture was sti...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Secondary amine
Tertiary amine.Sulfinate
null
C1COS[NH]1
C1COS[NH]1.c1ccncc1
HCl
ClCCl
null
0.5
C[C@H](CO)Nc1ccccn1.O=S(Cl)Cl>ClCCl>CC1CO[S@@](=O)N1c1ccccn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-894fd0022b9d41c08eca3c3e063480b8
CC1CO[S@@](=O)N1c1ccccn1.[O-][I+3]([O-])([O-])[O-]>>C[C@@H]1COS(=O)(=O)N1c1ccccn1
C(C)(=O)OCC.I(=O)(=O)(=O)[O-].[Na+].CC1N([S@@](OC1)=O)C1=NC=CC=C1>>C[C@H]1N(S(OC1)(=O)=O)C1=NC=CC=C1
[CH3:1][CH:2]1[CH2:3][O:4][S@@:5](=[O:7])[N:8]1[c:9]1[cH:10][cH:11][cH:12][cH:13][n:14]1.[O-][I+3]([O-])([O-])[O-:6]>>[CH3:1][C@@H:2]1[CH2:3][O:4][S:5](=[O:6])(=[O:7])[N:8]1[c:9]1[cH:10][cH:11][cH:12][cH:13][n:14]1
CC1CO[S@@](=O)N1c1ccccn1.[O-][I+3]([O-])([O-])[O-]
C[C@@H]1COS(=O)(=O)N1c1ccccn1
null
[Ru](Cl)(Cl)Cl
C(C)#N.O
Oxidation
OtherReaction
92d5ffa8b213dca13ca6074410126311038742783dec16e6a8042db63b59a05b
af0860f95582a26dccf6319bcb57e674f568c8c484a6a567b7d7bc738c3a91e4
O=S1(=O)OCCN1c1ccccn1
[#7;a:1]:[c:2]-[#7:3]1-[C:4]-[C:5]-[#8:6]-[S@;H0;D3;+0:7]-1=[O;D1;H0:8].[O-;H0;D1:9]-[I+3](-[O-])(-[O-])-[O-]>>[#7;a:1]:[c:2]-[#7:3]1-[C:4]-[C:5]-[#8:6]-[S;H0;D4;+0:7]-1(=[O;D1;H0:8])=[O;H0;D1;+0:9]
null
[]
null
null
null
null
A solution of sodium periodate (21 g, 0.10 moles) in water (150 ml) was added slowly to a solution of (R)-4-methyl-3-pyridin-2-yl-[1,2,3]oxathiazolidine-2-oxide (15.4 g, 0.78 moles) and ruthenium(III)chloride (20 mg) in acetonitrile (1540 ml) whilst the temperature was kept below 5° C. A heavy precipitate developed. Th...
10.6084/m9.figshare.5104873.v1
null
Sulfinate
Sulfamate
C1COS[NH]1
C1COS[NH]1
C1COS[NH]1.c1ccncc1
I-
[Ru](Cl)(Cl)Cl.C(C)#N.O
null
null
CC1CO[S@@](=O)N1c1ccccn1.[O-][I+3]([O-])([O-])[O-]>[Ru](Cl)(Cl)Cl.C(C)#N.O>C[C@@H]1COS(=O)(=O)N1c1ccccn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-094501f6e5574d25af8d8557ebfc848e
C[C@@H]1COS(=O)(=O)N1c1ccccn1.c1cc(N2CCNCC2)c2cc[nH]c2c1>>C[C@H](CN1CCN(c2cccc3[nH]ccc23)CC1)Nc1ccccn1
C[C@H]1N(S(OC1)(=O)=O)C1=NC=CC=C1.N1(CCNCC1)C1=C2C=CNC2=CC=C1>>N1C=CC2=C(C=CC=C12)N1CCN(CC1)C[C@H](NC1=NC=CC=C1)C
O=S1(=O)O[CH2:3][C@@H:2]([CH3:1])[N:19]1[c:20]1[cH:21][cH:22][cH:23][cH:24][n:25]1.[NH:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][cH:11][c:12]3[nH:13][cH:14][cH:15][c:16]23)[CH2:17][CH2:18]1>>[CH3:1][C@H:2]([CH2:3][N:4]1[CH2:5][CH2:6][N:7]([c:8]2[cH:9][cH:10][cH:11][c:12]3[nH:13][cH:14][cH:15][c:16]23)[CH2:17][CH2:18]1...
C[C@@H]1COS(=O)(=O)N1c1ccccn1.c1cc(N2CCNCC2)c2cc[nH]c2c1
C[C@H](CN1CCN(c2cccc3[nH]ccc23)CC1)Nc1ccccn1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
8f41d66678295c8bc94d7c54b6d59ad5ffb6169c1fa057a13b5d9d5cf8cd6ac9
599291d464aa192b54fe88259a98d054ef3f70cbce75e19456bd40be9dc0bc7b
c1ccc(NCCN2CCN(c3cccc4[nH]ccc34)CC2)nc1
O=S1(=O)-O-[CH2;D2;+0:1]-[C:2](-[C;D1;H3:3])-[N;H0;D3;+0:4]-1-[c:5](:[c:6]):[#7;a:7]:[c:8].[#7:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[C;D1;H3:3]-[C:2](-[CH2;D2;+0:1]-[N;H0;D3;+0:12]1-[C:11]-[C:10]-[#7:9]-[C:14]-[C:13]-1)-[NH;D2;+0:4]-[c:5](:[c:6]):[#7;a:7]:[c:8]
67.5
[{"value": 67.5, "product": "N1C=CC2=C(C=CC=C12)N1CCN(CC1)C[C@H](NC1=NC=CC=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
null
null
A solution of (R)-4-methyl-3-pyridin-2-yl-[1,2,3]-oxathiazolidine-2,2-dioxide (4.04 g 0.019 moles) and 4-piperazinoindole (3.80 g 0.019 moles) in acetonitrile (200 ml) was heated to 60° C. for 0.5 h then evaporated in vacuo. The residue was taken up into dilute HCl (100 ml), warmed to 60° C. for 0.5 h, cooled, washed w...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Tertiary amine.Sulfamate
Secondary amine.Tertiary amine
C1COS[NH]1.C1CNCC[NH]1
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1ccc2[nH]ccc2c1.c1ccncc1
Other
C(C)#N
60
null
C[C@@H]1COS(=O)(=O)N1c1ccccn1.c1cc(N2CCNCC2)c2cc[nH]c2c1>C(C)#N>C[C@H](CN1CCN(c2cccc3[nH]ccc23)CC1)Nc1ccccn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1d28f93300e04c54af211412e745642b
C[C@H](O)CN.Clc1ccccn1>>C[C@H](O)CNc1ccccn1
NC[C@H](C)O.CC(C)([O-])C.[K+].ClC1=NC=CC=C1>>N1=C(C=CC=C1)NC[C@H](C)O
[CH3:1][C@H:2]([OH:3])[CH2:4][NH2:5].Cl[c:6]1[cH:7][cH:8][cH:9][cH:10][n:11]1>>[CH3:1][C@H:2]([OH:3])[CH2:4][NH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][n:11]1
C[C@H](O)CN.Clc1ccccn1
C[C@H](O)CNc1ccccn1
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
c026a7bf7aba66b20cf21a13c528689aaaa1c05901524d62b36ca0c3b0572cef
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccncc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4]:[c:5]
84.4
[{"value": 84.4, "product": "N1=C(C=CC=C1)NC[C@H](C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
(S)-1-amino-2-propanol (43 g, 0.57M) was added to a stirred solution of potassium tertiary butoxide (64.2 g, 0.66M) in tetrahydrofuran (500 ml). 2-Chloropyridine (65.1 g 0.66M) was then added dropwise. After the exothermic reaction had subsided, the reaction was heated under reflux overnight, filtered to remove the pot...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccncc1
c1ccncc1
c1ccncc1
HCl
O1CCCC1
null
null
C[C@H](O)CN.Clc1ccccn1>O1CCCC1>C[C@H](O)CNc1ccccn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-3287b7f0e07644e393371b77d33adaf0
Nc1ccccn1.O=C(Cl)CCl>>O=C(CCl)Nc1ccccn1
ClCC(=O)Cl.NC1=NC=CC=C1.C(C)(C)N(CC)C(C)C>>ClCC(=O)NC1=NC=CC=C1
[NH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][n:11]1.Cl[C:2](=[O:1])[CH2:3][Cl:4]>>[O:1]=[C:2]([CH2:3][Cl:4])[NH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][n:11]1
Nc1ccccn1.O=C(Cl)CCl
O=C(CCl)Nc1ccccn1
null
null
ClCCl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccncc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[Cl;D1;H0:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[#7;a:8]:[c:9]>>[Cl;D1;H0:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[c:7]):[#7;a:8]:[c:9]
80.1
[{"value": 80.1, "product": "ClCC(=O)NC1=NC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Chloroacetylchloride (60 g, 0.53M) was added with stirring to a mixture of 2-aminopyridine (50 g, 0.53M) and diisopropylethylamine (75 ml, 0.53M) in dichloromethane (500 ml) keeping the temperature below 5° C. After the reaction mixture was warmed to room temperature it was filtered and washed with water. The organic l...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccncc1
HCl
ClCCl
null
null
Nc1ccccn1.O=C(Cl)CCl>ClCCl>O=C(CCl)Nc1ccccn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d2aea31453084c8dba037f866c0833b5
C1CNCCN1.COc1ccccc1C=CCO>>COc1ccccc1/C=C/CN1CCN(C/C=C/c2ccccc2OC)CC1
COC1=C(C=CCO)C=CC=C1.S(=O)(Cl)Cl.N1CCNCC1>>COC1=C(C=CC=C1)/C=C/CN1CCN(CC1)C\C=C\C1=C(C=CC=C1)OC
[CH2:1]1[CH2:8][NH:12][CH2:9][CH2:10][NH:15]1.[OH:2][CH2:16][CH:17]=[CH:18][c:19]1[cH:20][cH:21][cH:22][cH:23][c:24]1[O:25][CH3:26]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1/[CH:9]=[CH:10]/[CH2:11][N:12]1[CH2:13][CH2:14][N:15]([CH2:16]/[CH:17]=[CH:18]/[c:19]2[cH:20][cH:21][cH:22][cH:23][c:24]2[O:25][CH3:26])[CH...
C1CNCCN1.COc1ccccc1C=CCO
COc1ccccc1/C=C/CN1CCN(C/C=C/c2ccccc2OC)CC1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
ae38299a0dc1b7d9b40bbb5e2efe189375071b36bd4710814491a861f49ebbcd
67bf8e269000e5e8ec7808c6cda59bc0898ee178a898a68ad64a0f0c67a170be
C(=C/c1ccccc1)\CN1CCN(C/C=C/c2ccccc2)CC1
[CH2;D2;+0:1]1-[CH2;D2;+0:2]-[NH;D2;+0:3]-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[NH;D2;+0:6]-1.[OH;D1;+0:7]-[CH2;D2;+0:8]-[C:9]=[C:10]-[c:11]>>[CH3;D1;+0:5]-[O;H0;D2;+0:7]-[c:12](:[c:13]):[c;H0;D3;+0:4](/[CH;D2;+0:2]=[CH;D2;+0:1]/[C:14]-[N;H0;D3;+0:3]1-[C:15]-[C:16]-[N;H0;D3;+0:6](-[CH2;D2;+0:8]/[C:9]=[C:10]/[c:11])-[C:17]-[C:18...
null
[]
null
null
null
null
2-Methoxy-cinnamylalcohol (1.44 g) was chlorinated using thionylchloride. Subsequently, reaction with piperazine and other treatments were performed as described in Preparation Example 2, to thereby obtain 314 mg of a salt as colorless prisms. Conditions: See reaction.notes.procedure_details. Workup: as described in Pr...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Secondary amine.Secondary amine
Ether.Tertiary amine.Tertiary amine
C1CNCCN1
c1ccccc1.C1C[NH]CC[NH]1
c1ccccc1.C1C[NH]CC[NH]1.c1ccccc1
Other
null
null
null
C1CNCCN1.COc1ccccc1C=CCO>>COc1ccccc1/C=C/CN1CCN(C/C=C/c2ccccc2OC)CC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-754d50c008364ac9b11186dee1fd24b1
CCOC(=O)C(=O)CBr.O=C1CCCCC1=O>>O=C(O)c1coc2c1C(=O)CCC2
[OH-].[Na+].[OH-].[K+].C1(C(CCCC1)=O)=O.BrCC(C(=O)OCC)=O>>O=C1CCCC2=C1C(=CO2)C(=O)O
CC[O:3][C:2](=[O:1])[C:4]([CH2:5]Br)=[O:6].O=[C:8]1[CH2:7][CH2:13][CH2:12][CH2:11][C:9]1=[O:10]>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][o:6][c:7]2[c:8]1[C:9](=[O:10])[CH2:11][CH2:12][CH2:13]2
CCOC(=O)C(=O)CBr.O=C1CCCCC1=O
O=C(O)c1coc2c1C(=O)CCC2
null
null
CO.O
Aromatic Heterocycle Formation
OtherReaction
12c523d95bc989e82a3c117bb5c0da9972d3a2503b927240d48f0eb0564d3e74
8131734fe6d69265d1a032be994ef2ac858280264b2f94ca2c209f0c391853b1
O=C1CCCc2occc21
Br-[CH2;D2;+0:1]-[C;H0;D3;+0:2](=[O;H0;D1;+0:3])-[C:4](=[O;D1;H0:5])-[O;H0;D2;+0:6]-C-C.O=[C;H0;D3;+0:7]1-[CH2;D2;+0:8]-[C:9]-[C:10]-[C:11]-[C:12]-1=[O;D1;H0:13]>>[O;D1;H0:13]=[C:12]1-[C:11]-[C:10]-[C:9]-[c;H0;D3;+0:8]2:[o;H0;D2;+0:3]:[cH;D2;+0:1]:[c;H0;D3;+0:2](-[C:4](=[O;D1;H0:5])-[OH;D1;+0:6]):[c;H0;D3;+0:7]:2-1
null
[]
0
CELSIUS
0.5
HOUR
4-Oxo-4,5,6,7-tetrahydrobenzofuran-3-carboxylic acid was prepared as follows: To a stirred solution of potassium hydroxide (28.06 g, 0.5 mol) in methyl alcohol (100 mL) under nitrogen at 0° C. was added dropwise a solution of cyclohexanedione (56.07 g, 0.5 mol) in methyl alcohol (100 mL). The mixture was stirred at 0° ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Ketone.Ketone.Ester
Carboxylic acid.Ketone
C1CCCCC1
c1cc2c(o1)CCCC2
c1cc2c(o1)CCCC2
HBr
CO.O
0
0.5
CCOC(=O)C(=O)CBr.O=C1CCCCC1=O>CO.O>O=C(O)c1coc2c1C(=O)CCC2
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ac1973ef2f974d578c8e88e00c27d930
CC(=O)Cl.O=C(O)c1coc2c1C(=O)CCC2>>CCOC(=O)c1coc2c1C(=O)CCC2
O=C1CCCC2=C1C(=CO2)C(=O)O.C(C)(=O)Cl>>O=C1CCCC2=C1C(=CO2)C(=O)OCC
O=[C:2](Cl)[CH3:1].[OH:3][C:4](=[O:5])[c:6]1[cH:7][o:8][c:9]2[c:10]1[C:11](=[O:12])[CH2:13][CH2:14][CH2:15]2>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][o:8][c:9]2[c:10]1[C:11](=[O:12])[CH2:13][CH2:14][CH2:15]2
CC(=O)Cl.O=C(O)c1coc2c1C(=O)CCC2
CCOC(=O)c1coc2c1C(=O)CCC2
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
e4e418517831e68b0ae6eff0e20954e6373d72ef6db8a62429d10c826be6ea2e
b1bbfb03e48869c16300667505b58de6f6c5a435aa2a615a319deee7cf33326a
O=C1CCCc2occc21
Cl-[C;H0;D3;+0:1](=O)-[C;D1;H3:2].[#8;a:3]:[c:4]:[c:5]-[C:6](=[O;D1;H0:7])-[OH;D1;+0:8]>>[#8;a:3]:[c:4]:[c:5]-[C:6](=[O;D1;H0:7])-[O;H0;D2;+0:8]-[CH2;D2;+0:1]-[C;D1;H3:2]
null
[]
null
null
1
HOUR
To a stirred suspension of 4-oxo-4,5,6,7-tetrahydrobenzofuran-3-carboxylic acid (28.2 g, 157 mmol) in ethyl alcohol (500 mL) under nitrogen at ambient temperature was added acetyl chloride(56 mL, 783 mmol) dropwise. After stirring 1 h, the solution was then heated at reflux for 1 h. The solution was cooled and concentr...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Carboxylic acid
Ester
null
null
c1cc2c(o1)CCCC2
Other
C(C)O
null
1
CC(=O)Cl.O=C(O)c1coc2c1C(=O)CCC2>C(C)O>CCOC(=O)c1coc2c1C(=O)CCC2