HRID64991

反应详情

EQUATION

反应方程式

HRID 64991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In a 500 ml, 3-necked flask was dissolved glycine (9.03 g) in water (50 ml). The flask was cooled in an ice/methanol bath. Sodium hydroxide (12.6 g) in 30 cc of water was added. 2-Trifluoromethylbenzoyl chloride (25 g) was added at a temperature below 0° C. The bath was removed and the reaction mixture stirred for 2.5 hours at room temperature. To this was added concentrated HCl until the pH was 1. The solid was collected by filtration, washed with water and dried to give 25 g(84%), m.p. 147°-149° C. The product was a single spot by thin layer chromatography. (n-butyl alcohol:isopropyl alcohol:NH4OH; 10:4:4).

WORKUP

后处理

  1. temperatureThe flask was cooled in an ice/methanol bath
  2. customThe bath was removed
  3. additionTo this was added concentrated HCl until the pH was 1
  4. filtrationThe solid was collected by filtration
  5. washwashed with water
  6. customdried
  7. customto give 25 g(84%), m.p. 147°-149° C