Methanol → Methyl 2,2-difluoro-4-hydroxybutanoate

HRID 2072876노트

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HRID 2072876 반응식
[F:1][C:2]([F:11])([CH2:7][C:8]([O-])=[O:9])[C:3]([O:5][CH3:6])=[O:4].CO>O1CCCC1>[F:1][C:2]([F:11])([CH2:7][CH2:8][OH:9])[C:3]([O:5][CH3:6])=[O:4]

참가 물질

4

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온도
80 °C

실험 절차

In a 4 L flask equipped with a reflux condenser and 1 L dropping funnel, a solution of BH3.Me2S complex (10M, 88 mL) in dry dicholoromethane (1 L) is slowly added over a 2 hour period to a stirred solution of the methyl 2,2-difluorosuccinate (120 g, 0.714 moles) in dry tetrahydrofuran at 20° C. After refluxing (bath temperature 80° C.) for about 15 hours, the mixture is allowed to cool to room temperature and methanol (1 L) is slowly added. Evaporation yields methyl 2,2-difluoro-4-hydroxybutyrate as an oil which is stripped with methanol (1 L) and finally with CCl4 to yield a yellow oil: 100 g (92%).

후처리

  1. customIn a 4 L flask equipped with a reflux condenser
  2. temperatureto cool to room temperature
  3. customEvaporation

출처 및 근거

ORD 기록
ord-8025c91ea344477c97fde37078da9f3d
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04914240

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