HRID232153

反应详情

EQUATION

反应方程式

HRID 232153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of bromo-(4-chlorophenyl)hydrazonoacetic acid ethyl ester (18.24 g, 60 mmol) in toluene (390 ml) and 10.02 g (60 mmol) of morpholinocyclohexene (10.02 g, 60 mmol) was cooled to 0° C. and triethylamine (12.6 ml, 90 mmol) was added. The solution was reacted for 1.5 hours at 0° C. and at ambient temperature for 48 hours. Triethylamine hydrochloride was filtered, the filtrate was washed with 10% hydrochloric acid, dried and evaporated. The crude product was crystallized from methanol to yield pure title compound (10.04 g), m.p. 139°-140° C. (lit 139°-141° C.).

WORKUP

后处理

  1. customThe solution was reacted for 1.5 hours at 0° C. and at ambient temperature for 48 hours
  2. filtrationTriethylamine hydrochloride was filtered
  3. washthe filtrate was washed with 10% hydrochloric acid
  4. customdried
  5. customevaporated
  6. customThe crude product was crystallized from methanol