3-(Trifluoromethyl)phenyl isocyanate → N-[3-(trifluoromethyl)phenyl]-1,3,4,9-tetrahydro-2H-beta-carboline-2-carboxamide

HRID 253731ノート

反応式

HRID 253731 の反応式
[CH2:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH2:4][CH2:3][NH:2]1.[N:14]([C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=1)=[C:15]=[O:16]>CN(C)C=O.ClCCl>[F:24][C:23]([F:25])([F:26])[C:19]1[CH:18]=[C:17]([NH:14][C:15]([N:2]2[CH2:3][CH2:4][C:5]3[C:6]4[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=4)[NH:12][C:13]=3[CH2:1]2)=[O:16])[CH:22]=[CH:21][CH:20]=1

参加物

5

反応物 2

HCID 94833-(Trifluoromethyl)phenyl isocyanateHCID 107838Tetrahydro-beta-carboline

生成物 1

HCID 23113599N-[3-(trifluoromethyl)phenyl]-1,3,4,9-tetrahydro-2H-beta-carboline-2-carboxamide収率 61.7%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 2,3,4,9-tetrahydro-1H-β-carboline (172 mg) in dimethylformamide (5 mL) was added by a solution of 1-isocyanato-3-(trifluoromethyl)benzene (173 mg) in dichloromethane (5 mL) and stirred overnight at the room temperature. The mixture was concentrated under reduced pressure and the residue was purified by column chromatography on silica gel (hexane:ethyl acetate=6:1) to give the title compound (205 mg) having the following physical data.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customthe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=6:1)

出典と根拠

ORDレコード
ord-9ebe548c246e451ab7c77a5d5b14032b
出典データセット
uspto-grants-2011_01
特許番号
US07872133B2

反応ノート

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