HRID64991
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe flask was cooled in an ice/methanol bath
- customThe bath was removed
- additionTo this was added concentrated HCl until the pH was 1
- filtrationThe solid was collected by filtration
- washwashed with water
- customdried
- customto give 25 g(84%), m.p. 147°-149° C