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

HRID 891955노트

반응식

HRID 891955 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

HCID 2224027066351-92-6수율 76%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

반응 조건

온도
115 °C

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-9d5bf4bd1bef44b2a6acbe1fbb7d4dd3
출처 데이터셋
uspto-grants-2006_02
특허 번호
US07005432B2

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