HRID369077
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
- 60 °C
PROCEDURE
实验过程
A mixture of (R)-glycidyl 4-toluenesulphonate (24 g), 5-trifluoromethyl-2-hydroxybenzaldehyde (20 g) and potassium carbonate (16 g) in dimethylformamide (550 ml) was stirred and heated at 60° C. for 72 hours. After cooling, brine (1.5 L) was added and the resultant mixture extracted with ether (4×500 ml). The combined ether extracts were washed with brine (2×500 ml), then water (500 ml) and dried over magnesium sulphate. The residue was purified by flash column chromatography on silica eluting with a 3:1 mixture of petroleum ether (b.p. 40-60 ° C.) and ethyl acetate to give (R)-5-trifluoromethyl-2-(2,3-epoxypropoxy)benzaldehyde (18.7 g) as a yellow oil.
WORKUP
后处理
- temperatureAfter cooling
- extractionthe resultant mixture extracted with ether (4×500 ml)
- washThe combined ether extracts were washed with brine (2×500 ml)
- dry with materialwater (500 ml) and dried over magnesium sulphate
- customThe residue was purified by flash column chromatography on silica eluting with a 3:1 mixture of petroleum ether (b.p. 40-60 ° C.) and ethyl acetate