HRID231046

反应详情

EQUATION

反应方程式

HRID 231046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

To a solution of iso-butyric acid (1.6 ml) in THF (10 ml) at 0° C. was added Et3N (2.7 ml) and methylchloroformate (1.5 ml). To this resulting suspension was added slowly at 0° C. a solution of 4-chloro-3-hydroxy-10H-phenothiazine in THF (10 ml). The reaction mixture was stirred at 5° C. for 12 hours, after which H2O was added and the resulting aqueous phase extracted with ethyl acetate. The organic layer was then dried and evaporated. The resulting residue was purified by chromatography on silica gel to give 2.25 g of 4-chloro-3-isobutyryloxy-10H-phenothiazine (m.p. 155° C.).

WORKUP

后处理

  1. extractionthe resulting aqueous phase extracted with ethyl acetate
  2. customThe organic layer was then dried
  3. customevaporated
  4. customThe resulting residue was purified by chromatography on silica gel