1-Chloro-2-(difluoromethyl)-4-nitrobenzene → 66351-92-6

HRID 891955ノート

反応式

HRID 891955 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-])=O)=[CH:4][C:3]=1[CH:11]([F:13])[F:12]>C(O)(=O)C.[Fe]>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[CH:4][C:3]=1[CH:11]([F:12])[F:13]

参加物

4

反応物 1

HCID 222401911-Chloro-2-(difluoromethyl)-4-nitrobenzene

生成物 1

HCID 2224027066351-92-6収率 76%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

反応条件

温度
115 °C

実験手順

To a suspension of iron powder (16 g) in acetic acid (95 ml) was added 1-chloro-2-difluoromethyl-4-nitro-benzene (5.1 g, 15 mmol) and the reaction mixture was heated to 115° C. for 15 minutes. The mixture was filtered and the residue was washed with acetic acide and CH2Cl2. Evaporation of the solvent gave the crude product. It was further purified by chromatography over silica gel to give 4-chloro-3-difluoromethyl-phenylamine (76%), MS: m/e=177.1 (M+).

後処理

  1. filtrationThe mixture was filtered
  2. washthe residue was washed with acetic acide and CH2Cl2
  3. customEvaporation of the solvent
  4. customgave the crude product
  5. customIt was further purified by chromatography over silica gel

出典と根拠

ORDレコード
ord-9d5bf4bd1bef44b2a6acbe1fbb7d4dd3
出典データセット
uspto-grants-2006_02
特許番号
US07005432B2

反応ノート

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