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

HRID 221832ノート

反応式

HRID 221832 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b7f24d533f3446208c74a6c4dcfea0bb
出典データセット
uspto-grants-2012_06
特許番号
US08207168B2

反応ノート

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