HCID 23359001、化合物 → HCID 23359007、化合物

HRID 232647ノート

反応式

HRID 232647 の反応式
[F:1][C:2]1[C:8]([CH3:9])=[C:7]([F:10])[C:6]([F:11])=[C:5]([CH2:12]SC)[C:3]=1[NH2:4]>[Ni].C(O)C>[F:1][C:2]1[C:8]([CH3:9])=[C:7]([F:10])[C:6]([F:11])=[C:5]([CH3:12])[C:3]=1[NH2:4]

参加物

4

反応物 1

HCID 23359001HCID 23359001、化合物

生成物 1

HCID 23359007HCID 23359007、化合物収率 69.7%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

To 2,4,5-trifluoro-3-methyl-6-methylthiomethylaniline (10.67 g) are added ethanol (300 ml) and Raney nickel (100 g, wet) and the mixture is stirred at room temperature for 30 minutes. After Raney nickel is filtered off, the filtrate is concentrated, diluted with water, extracted with dichloromethane, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and the residue is purified by silica-gel column-chromatography (dichloromethane: n-hexane =1:1) to give 2,4,5-trifluoro-3,6-dimethylaniline (5.89 g), as yellow crystals.

後処理

  1. filtrationAfter Raney nickel is filtered off
  2. concentrationthe filtrate is concentrated
  3. additiondiluted with water
  4. extractionextracted with dichloromethane
  5. washthe extract is washed with water
  6. customdried
  7. distillationThe solvent is distilled off under reduced pressure
  8. customthe residue is purified by silica-gel column-chromatography (dichloromethane: n-hexane =1:1)

出典と根拠

ORDレコード
ord-de76bd3b62474e8bb2457160fa994382
出典データセット
uspto-grants-1997_01
特許番号
US05591744

反応ノート

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