HRID1197321
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
PROCEDURE
实验过程
2-Benzyloxymethyl-2-cyclohexyl-propan-1,3-diol (5.5 g.) in dry diethyl ether (50 ml.) was added to liquid ammonia (200 ml) at -70°. Sodium (2.5 g.) was added to the stirred solution. Stirring was maintained at -70°, for 1 hour. The mixture was allowed to warm up to 0° and solid ammonium chloride (15 g.) was added cautiously. The ammonia was removed from the reaction mixture under a current of nitrogen. Methanol (25 ml.) was added to the stirred mixture to destroy residual sodium. Dichloromethane (400 ml) was added and the mixture was filtered. The filtrates were evaporated in vacuo. 2-Cyclohexyl-2-hydroxymethylpropan-1,3-diol was obtained as a colourless solid (3.2 g.).
WORKUP
后处理
- temperaturewas maintained at -70°, for 1 hour
- temperatureto warm up to 0°
- customThe ammonia was removed from the reaction mixture under a current of nitrogen
- additionMethanol (25 ml.) was added to the stirred mixture
- customto destroy residual sodium
- additionDichloromethane (400 ml) was added
- filtrationthe mixture was filtered
- customThe filtrates were evaporated in vacuo