HRID1707519

反应详情

EQUATION

反应方程式

HRID 1707519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureit was refluxed for 2 hours in a hot water bath
  2. extractionit was extracted with chloroform
  3. washwashed in 10% HC1 and water
  4. customThe chloroform was removed
  5. distillationthe remaining oily substance was distilled under reduced pressure (b. p. 110° C./4 mmHg)