HRID542986

反应详情

EQUATION

反应方程式

HRID 542986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of glycine (15 g, 0.2 mol) in 175 mL of 5% aqueous sodium hydroxide is cooled to 10° C. to 15° C. p-Fluorobenzoyl chloride (31.6 g, 0.2 mol) is then added, dropwise, to the mixture and stirred vigorously for 0.5 hour, while maintaining the temperature of the mixture at about 10° C. to 15° C. The pH of the reaction mixture is maintained at pH>9 by the dropwise addition at 50% aqueous sodium hydroxide. The mixture is stirred at 10° C. to 15° C. for two hours with the resulting clear solution then acidified with concentrated HCl to pH=1. The resulting product is filtered off, washed with water (2×100 mL) and air dried to give a white solid (30.8 g, 78.1%); mp=161°-163° C.

WORKUP

后处理

  1. additionis then added
  2. temperaturewhile maintaining the temperature of the mixture at about 10° C. to 15° C
  3. stirringThe mixture is stirred at 10° C. to 15° C. for two hours with the resulting clear solution
  4. filtrationThe resulting product is filtered off
  5. washwashed with water (2×100 mL) and air
  6. customdried