HRID1654181
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
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.
WORKUP
后处理
- distillationMethanol was distilled off under reduced pressure
- extractionThe residue was subjected to extraction by the addition of ethyl acetate (700 ml) and water (500 ml)
- dry with materialThe ethyl acetate layer was dried over magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was crystallized from hexane (200 ml)