HRID1707519
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
34 g (0.9 mol) of LiAlH4 was dispersed in 690 cm3 of anhydrous THF, and 159 g (0.69 mol) of diethyl pentylmalonate was added dropwise under stirring. After the dropping was completed, it was refluxed for 2 hours in a hot water bath, and after cooling to room temperature, the excess LiAlH4 was decomposed by dropwise addition of THF including 10% water. 500 cm3 of concentrated hydrochloric acid was added, it was extracted with chloroform and washed in 10% HC1 and water. The chloroform was removed, and the remaining oily substance was distilled under reduced pressure (b. p. 110° C./4 mmHg) to obtain 76 g (0.52 mol) of 2-pentylpropane-1,3diol).
WORKUP
后处理
- temperatureit was refluxed for 2 hours in a hot water bath
- extractionit was extracted with chloroform
- washwashed in 10% HC1 and water
- customThe chloroform was removed
- distillationthe remaining oily substance was distilled under reduced pressure (b. p. 110° C./4 mmHg)