HRID1589739

反应详情

EQUATION

反应方程式

HRID 1589739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

100 cm3 of toluene was added to 170 cm3 (0.6 mol) of 70% toluene solution of NaAlH2 (OC2H4OCH3)2. 133 g (0.50 mol) of 4-(trans-4'-propylcyclohexyl) benzoic acid chloride was added drop-wise to the solution while stirring at a rate to moderately reflux the toluene solution and the mixture was stirred over a warm water bath at a temperature of 88°-90° C. for 5 hours. The solution was cooled to room temperature and 500 cm3 of concentrated hydrochloric acid diluted by twice its volume was added drop-wise. The toluene layer was separated out and the aqueous layer was extracted three times with 100 cm3 of toluene. The toluene layers were combined and washed with 10% hydrochloric acid and water. The toluene was distilled off under reduced pressure and the residue was distilled under reduced pressure (150° C./2.5 mmHg) to yield 114 g (0.49 mol) of 4-(trans-4'-propylcyclohexyl) benzyl alcohol.

WORKUP

后处理

  1. stirringthe mixture was stirred over a warm water bath at a temperature of 88°-90° C. for 5 hours
  2. additionwas added drop-wise
  3. customThe toluene layer was separated out
  4. extractionthe aqueous layer was extracted three times with 100 cm3 of toluene
  5. washwashed with 10% hydrochloric acid and water
  6. distillationThe toluene was distilled off under reduced pressure
  7. distillationthe residue was distilled under reduced pressure (150° C./2.5 mmHg)