HRID2254941

反应详情

EQUATION

反应方程式

HRID 2254941 反应方程式

PROCEDURE

实验过程

A mixture of 31 g (0.17 mol) of 2-(trans-4'-butylcyclohexyl) ethanol and 14 g (0.18 mol) of anhydrous pyridine was stirred over an ice water bath and 25 g (0.21 mol) of SOCl2 was added drop-wise to the mixture. The resulting reaction product was stirred and heated with a mantle heater at 105° to 110° C. for 3 hours. The reaction product was cooled to room temperature and poured into a beaker containing ice and concentrated hydrochloric acid. The oily layer was separated out and the aqueous layer was extracted with chloroform. The two layer were combined and washed with an aqueous 10% hydrochloric acid solution and water. The chloroform was distilled off. The residual liquid was distilled in a vacuum (b.p. 96° C./3 mmHg) to yield 30 g (0.15 mol) of 2-(trans-4'-butylcyclohexyl)-1-chloroethane.

WORKUP

后处理

  1. customThe resulting reaction product
  2. stirringwas stirred
  3. temperatureheated with a mantle heater at 105° to 110° C. for 3 hours
  4. additionpoured into a beaker
  5. customThe oily layer was separated out
  6. extractionthe aqueous layer was extracted with chloroform
  7. washwashed with an aqueous 10% hydrochloric acid solution and water
  8. distillationThe chloroform was distilled off
  9. distillationThe residual liquid was distilled in a vacuum (b.p. 96° C./3 mmHg)