Hydrogen Bromide → 1-(3,5-Difluoro-4-hydroxyphenyl)ethan-1-one

HRID 221832노트

반응식

HRID 221832 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:11](=[O:13])[CH3:12])[CH:5]=[C:6]([F:10])[C:7]=1[O:8]C.Br>O>[F:1][C:2]1[CH:3]=[C:4]([C:11](=[O:13])[CH3:12])[CH:5]=[C:6]([F:10])[C:7]=1[OH:8]

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 27369833',5'-Difluoro-4'-methoxyacetophenone

생성물 1

HCID 151513381-(3,5-Difluoro-4-hydroxyphenyl)ethan-1-one수율 91%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1-(3,5-difluoro-4-methoxyphenyl)ethanone (12 g, 64.5 mmol) and 48% aqueous HBr (32 mL) was stirred at reflux for 30 h. The reaction was cooled to rt and diluted with water and the aqueous layer was extracted twice with methylene chloride. The combined organics were dried (Na2SO4), filtered, and concentrated to give 1-(3,5-difluoro-4-hydroxyphenyl)ethanone (10 g, 91%), mp 141-143° C.; MS m/z 171 (M−H).

후처리

  1. temperatureat reflux for 30 h
  2. extractionthe aqueous layer was extracted twice with methylene chloride
  3. dry with materialThe combined organics were dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b7f24d533f3446208c74a6c4dcfea0bb
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207168B2

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