Sodium Formate → HCID 11830128, 화합물

HRID 1654181

반응식

HRID 1654181 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 11830128HCID 11830128, 화합물수율 47.9%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e423fc196af7458b83ca05fe6d3ebaca
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05405861

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