Hydrochloric Acid → 1-(4-Bromo-2,5-difluorophenyl)ethan-1-one

HRID 1957483노트

반응식

HRID 1957483 반응식
[C:1](Cl)(=[O:3])[CH3:2].[Br:5][C:6]1[CH:11]=[C:10]([F:12])[CH:9]=[CH:8][C:7]=1[F:13].[Cl-].[Cl-].[Cl-].[Al+3].Cl>>[Br:5][C:6]1[C:7]([F:13])=[CH:8][C:9]([C:1](=[O:3])[CH3:2])=[C:10]([F:12])[CH:11]=1

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 678622-Bromo-1,4-difluorobenzeneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 99916531-(4-Bromo-2,5-difluorophenyl)ethan-1-one

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온도
60 °C

실험 절차

Acetyl chloride (17 ml) is slowly dropped into a stirred mixture of 1-bromo-2,5-difluorobenzene (30 g) and aluminium trichloride (53 g) heated at 60° C. and kept under argon. The reaction mixture is then stirred 90 minutes at 95° C. The mixture is cooled at 40° C. and carefully poured into crushed ice (400 g) and concentrated hydrochloric acid (35 ml). The resulting mixture is stirred a few minutes and then extracted with ethyl ether (2×250 ml). The ethereal solution is washed to neutral with brine, dried over sodium sulfate and the solvent is evaporated. The distillation of the oily residue gives 4'-bromo-2 ',5'-difluoroacetophenone (21.2 g) b.p. (0.05 mm)=60° C.

후처리

  1. temperatureThe mixture is cooled at 40° C.
  2. additioncarefully poured
  3. stirringThe resulting mixture is stirred a few minutes
  4. extractionextracted with ethyl ether (2×250 ml)
  5. washThe ethereal solution is washed to neutral with brine
  6. dry with materialdried over sodium sulfate
  7. customthe solvent is evaporated
  8. distillationThe distillation of the oily residue

출처 및 근거

ORD 기록
ord-198b147a0184444fb062f6bd53d235b0
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05786350

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