N-cyclohexyl-N-methyl-2-nitrobenzamide → 2-amino-N-cyclohexyl-N-methylbenzamide

HRID 852234ノート

反応式

HRID 852234 の反応式
[CH:1]1([N:7]([CH3:19])[C:8](=[O:18])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N+:15]([O-])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1>CO.[Ni]>[NH2:15][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[C:8]([N:7]([CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)[CH3:19])=[O:18]

参加物

4

反応物 1

HCID 799283N-cyclohexyl-N-methyl-2-nitrobenzamide

生成物 1

HCID 8453022-amino-N-cyclohexyl-N-methylbenzamide収率 96%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

A solution of the crude N-cyclohexyl-N-methyl-2-nitrobenzamide (1.05 g, 4 mmol) and a catalytic amount of Raney-Ni® in methanol (25 ml) was stirred overnight under hydrogen at room temperature. The catalyst was removed by filtration and the filtrate was concentrated under reduced pressure. The resulting crude was dissolved in dichloromethane and washed with saturated aqueous sodium bicarbonate. The organic layer was dried (MgSO4) and the solvents removed under reduced pressure to give (0.89 g, 96%) of the title compound as a white solid.

後処理

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. dissolutionThe resulting crude was dissolved in dichloromethane
  4. washwashed with saturated aqueous sodium bicarbonate
  5. dry with materialThe organic layer was dried (MgSO4)
  6. customthe solvents removed under reduced pressure

出典と根拠

ORDレコード
ord-681d2c642a5d45a682ebb157387e4e2e
出典データセット
uspto-grants-2007_08
特許番号
US07253171B2

反応ノート

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