Sodium Formate → HCID 11830128、化合物

HRID 1654181

反応式

HRID 1654181 の反応式
Br[CH:2]([CH3:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[F:12])=[O:4].C([O-])=[O:15].[Na+]>CO>[F:12][C:6]1[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:5]=1[C:3](=[O:4])[CH:2]([OH:15])[CH3:13]

参加物

4

反応物 2

HCID 2723810Sodium FormateHCID 110758302-Bromo-1-(2,4-difluorophenyl)propan-1-one

生成物 1

HCID 11830128HCID 11830128、化合物収率 47.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

2-Bromo-2',4'-difluoropropiophenone (141 g) was dissolved in methanol (1100 ml), to which was added sodium formate (176.2 g), and the mixture was stirred for 2 days at 50° C. Methanol was distilled off under reduced pressure. The residue was subjected to extraction by the addition of ethyl acetate (700 ml) and water (500 ml). The ethyl acetate layer was dried over magnesium sulfate, then the solvent was distilled off under reduced pressure. The residue was crystallized from hexane (200 ml) to afford 2',4'-difluoro-2-hydroxypropiophenone (50.5 g) as colorless prisms, m.p. 49°-51° C.

後処理

  1. distillationMethanol was distilled off under reduced pressure
  2. extractionThe residue was subjected to extraction by the addition of ethyl acetate (700 ml) and water (500 ml)
  3. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was crystallized from hexane (200 ml)

出典と根拠

ORDレコード
ord-e423fc196af7458b83ca05fe6d3ebaca
出典データセット
uspto-grants-1995_04
特許番号
US05405861

関連ノート

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