HRID2254938

反应详情

EQUATION

反应方程式

HRID 2254938 反应方程式

PROCEDURE

实验过程

Over an ice water bath, 37 g (0.22 mol) of trans-4-butylcyclohexyl methanol and 18 g (0.23 mol) of anhydrous pyridine were stirred and 32 g (0.27 mol) of SOCl2 was added drop-wise to the mixture. The resulting reaction product was stirred on a mantle heater at a temperature of between about 105 and 110° C. for 3 hours. The reaction product was cooled to room temperature and poured into a breaker containing concentrated hydrochloric acid and ice. The oily layer was separated out and the aqueous layer was extracted with chloroform. The two layers were combined and washed with an aqueous 10% hydrochloric acid solution and water. The chloroform was distilled off. The oily residue was distilled in a vacuum (b.p. 80° C./3 mmHg) to yield 38 g (0.20 mol) of trans-4-butylcyclohexyl chloromethane.

WORKUP

后处理

  1. customThe resulting reaction product
  2. additionpoured into a breaker
  3. customThe oily layer was separated out
  4. extractionthe aqueous layer was extracted with chloroform
  5. washwashed with an aqueous 10% hydrochloric acid solution and water
  6. distillationThe chloroform was distilled off
  7. distillationThe oily residue was distilled in a vacuum (b.p. 80° C./3 mmHg)