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Dimethylformamide → 3-Chloro-2-fluoro-5-(trifluoromethyl)benzamide

HRID 1614414
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HRID 1614414 반응식
S(Cl)(Cl)=O.[Cl:5][C:6]1[C:7]([F:19])=[C:8]([CH:12]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:14]=1)[C:9](O)=[O:10].C[N:21](C)C=O>>[Cl:5][C:6]1[C:7]([F:19])=[C:8]([CH:12]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:14]=1)[C:9]([NH2:21])=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 27737513-Chloro-2-fluoro-5-(trifluoromethyl)benzoic acid

생성물 1

HCID 27737463-Chloro-2-fluoro-5-(trifluoromethyl)benzamide수율 99%

반응 조건

온도
75 °C

실험 절차

Thionyl chloride, 6.0 g (50 mmol) was added to a solution of 4.0 g (16 mmol) 3-chloro-2-fluoro-5-(trifluoromethyl) benzoic acid in 10 mL dimethylformamide. The reaction mixture was heated to 75° C. for 2 hours, cooled to room temperature and carefully added to 25 mL of ice cold ammonium hydroxide. The mixture was cooled to 0° C. and the solid product filtered, washed with water and dried to yield 3.96 g (99%) of 3-chloro-2-fluoro-5-(trifluoromethyl)benzamide.

후처리

  1. temperaturecooled to room temperature
  2. temperatureThe mixture was cooled to 0° C.
  3. filtrationthe solid product filtered
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-34197cc3bbb645eea9c61c672de4193a
출처 데이터셋
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05196593

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