HRID4704

反应详情

EQUATION

反应方程式

HRID 4704 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 of about 10° C. to 15° C. The pH of the reaction mixture is maintained at pH>9 by the dropwise addition of 50% aqueous sodium hydroxide. The mixture is stirred at 10° C. to 15° C. for two hours and the resulting clear solution then acidified to pH-1 with concentrated HCl. 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 dropwise to the mixture
  2. temperaturewhile maintaining
  3. additionthe temperature of the mixture of about 10° C. to 15° C
  4. stirringThe mixture is stirred at 10° C. to 15° C. for two hours
  5. filtrationThe resulting product is filtered off
  6. washwashed with water (2×100 mL) and air
  7. customdried