Methanol → Methyl 2,2-difluoro-4-hydroxybutanoate
반응식
[F:1][C:2]([F:11])([CH2:7][C:8]([O-])=[O:9])[C:3]([O:5][CH3:6])=[O:4].CO>ClCCl.O1CCCC1>[F:1][C:2]([F:11])([CH2:7][CH2:8][OH:9])[C:3]([O:5][CH3:6])=[O:4]참가 물질
5
반응 조건
- 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 dichloromethane (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
- customIn a 4 L flask equipped with a reflux condenser
- temperatureto cool to room temperature
- customEvaporation
출처 및 근거
- ORD 기록
- ord-f75ba9e36cc94fbe84b85d15545c455c
- 출처 데이터셋
- uspto-grants-1988_01
- 특허 번호
- US04719313
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