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Water → 3-Bromo-2-chloro-4,5-difluorobenzoic acid

HRID 414368
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HRID 414368 반응식
[Br:1][C:2]1[C:3]([Cl:12])=[C:4]([CH:7]=[C:8]([F:11])[C:9]=1[F:10])[C:5]#N.[OH2:13].S(=O)(=O)(O)[OH:15]>>[Br:1][C:2]1[C:3]([Cl:12])=[C:4]([CH:7]=[C:8]([F:11])[C:9]=1[F:10])[C:5]([OH:15])=[O:13]
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참가 물질

4

반응물 3

HCID 962WaterHCID 1118Sulfuric Acid2회HCID 140717963-Bromo-2-chloro-4,5-difluorobenzonitrile

생성물 1

HCID 98383473-Bromo-2-chloro-4,5-difluorobenzoic acid

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온도
100 °C

실험 절차

A solution of 3-bromo-2-chloro-4,5-difluorobenzonitrile (9.8 g) in concentrated sulfuric acid (10 ml) was stirred at 100° C. for 35 minutes. After cooling, 18N sulfuric acid (50 ml) and water (10 ml) were added to the reaction mixture. The reaction mixture was stirred at 100° C. for 4 hours and then poured into ice water (300 ml). The resulting precipitate was collected by filtration, washed with water sufficiently and recrystallized from dichloromethane-n-hexane to give the title compound (9.24 g) as colorless prisms, mp 137.5°-139.5 ° C.

후처리

  1. temperatureAfter cooling
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water sufficiently
  4. customrecrystallized from dichloromethane-n-hexane

출처 및 근거

ORD 기록
ord-de8ff113b7c54382ba5b6290bc363e9a
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04791225

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