HCID 23359035、化合物 → 2,4-Difluoro-3,6-dimethylaniline

HRID 2396946ノート

反応式

HRID 2396946 の反応式
[F:1][C:2]1[C:8]([CH3:9])=[C:7]([F:10])[CH:6]=[C:5]([CH2:11]SC)[C:3]=1[NH2:4]>[Ni].C(O)C>[F:1][C:2]1[C:8]([CH3:9])=[C:7]([F:10])[CH:6]=[C:5]([CH3:11])[C:3]=1[NH2:4]

参加物

4

反応物 1

HCID 23359035HCID 23359035、化合物

生成物 1

HCID 233590392,4-Difluoro-3,6-dimethylaniline収率 84.8%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒2 回

実験手順

To a solution of Raney nickel (50 g) in ethanol (100 ml) is added a solution of 2,4-difluoro-3-methyl-6-methylthiomethylaniline (4.79 g) in ethanol (30 ml) at room temperature with stirring, followed by stirring at room temperature for 30 minutes. The Raney nickel is filtered off and the filtrate is diluted with water, extracted with dichloromethane, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure to give 2,4-difluoro-3,6-dimethylaniline (3.14 g).

後処理

  1. stirringby stirring at room temperature for 30 minutes
  2. filtrationThe Raney nickel is filtered off
  3. additionthe filtrate is diluted with water
  4. extractionextracted with dichloromethane
  5. washthe extract is washed with water
  6. customdried
  7. distillationThe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-9a67ef943f4a41dda8fe431ef3c3754e
出典データセット
uspto-grants-1996_02
特許番号
US05495020

反応ノート

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