HRID1076766

反应详情

EQUATION

反应方程式

HRID 1076766 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15 g of 1-phenyl-2-hydroxy-cyclohex-3-ene-1-carboxylic-acid-ethyl-ester and 15 cc. of thionyl chloride and 1 cc. of dimethylformamide are heated under reflux for 10 minutes. Then direct distillation is done. 12.2 g of 1-phenyl-2-chloro-cyclohex-3-ene-1-carboxylic-acid-ethyl-ester of the boiling point 0.1/122°-5°C are obtained. By reacting with 12 g of β-phenylethyl amine in 100 cc. of DMSO for 2 hrs. at 100°C, processing as described above, 6.0 g of hydrochloride m.p. 179°-82°C are obtained.

WORKUP

后处理

  1. temperatureunder reflux for 10 minutes
  2. distillationThen direct distillation