HRID1417722

反应详情

EQUATION

反应方程式

HRID 1417722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of glycinamide hydrochloride (5.5 g), triethyl amine (5.05 g), 5-chloro-2-methoxyphenyl-isothiocyanate (9.95 g), and chloroform (500 mL) were heated at reflux for 3 hours. The mixture was then cooled to ambient temperature and washed with water (300 mL). The organic phase was separated. Precipitate formed upon standing. The solid was collected by filtration, washed with water, then with diethyl ether and air dried to give 2-[3-(5-chloro-2-methoxyphenyl)-thioureido]-acetamide (12.8 g), m.p. 166°-169° C. (dec.). This compound was used without further purification for the preparation of the title compound.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureat reflux for 3 hours
  3. washwashed with water (300 mL)
  4. customThe organic phase was separated
  5. customPrecipitate formed
  6. filtrationThe solid was collected by filtration
  7. washwashed with water
  8. dry with materialwith diethyl ether and air dried