HRID543247

反应详情

EQUATION

反应方程式

HRID 543247 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

50 g (0.113 mol) of the previously obtained dicyclohexylamine salt of N-benzyloxycarbonyl-(L)-pyroglutamic acid are mixed to a paste with 1 liter of toluene, 110 ml of thionyl chloride are run in dropwise and the temperature is then raised to 60° C. for 2 hours. The mixture is cooled and filtered, the filtrate is evaporated and the residue is taken up several times with benzene. The acid chloride finally crystallizes from petroleum ether with a practically quantitative yield. Melting point=65°-70° C. (literature=71/72° C.).

WORKUP

后处理

  1. temperatureThe mixture is cooled
  2. filtrationfiltered
  3. customthe filtrate is evaporated
  4. customThe acid chloride finally crystallizes from petroleum ether with a practically quantitative yield
  5. customMelting point=65°-70° C. (literature=71/72° C.)