HRID1698871

反应详情

EQUATION

反应方程式

HRID 1698871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At 0° C., under an inert atmosphere, 320 mg of 4-(2-chloro-4-methoxyphenyl)-5-methyl-2-[N-(5-hydroxymethyl-2-methoxyphenyl)-N-propylamino]thiazole are dissolved in 0.7 ml of dimethylformamide. 70 mg of sodium hydride (50% in oil) are added. After 5 minutes, 0.24 ml of methyl iodide is added. After 12 hours at room temperature, the reaction mixture is diluted with ethyl acetate and then hydrolyzed. The organic phase is washed several times with water before being dried over sodium sulphate. After purification on a silica gel; the expected product is dissolved in dichloromethane. A 0.1 N solution of hydrochloric acid in isopropanol is then added. After evaporation under vacuum, the expected product is obtained in hydrochloride form; m.p.=71° C.

WORKUP

后处理

  1. waitAfter 12 hours at room temperature
  2. washThe organic phase is washed several times with water
  3. dry with materialbefore being dried over sodium sulphate
  4. customAfter purification on a silica gel
  5. dissolutionthe expected product is dissolved in dichloromethane
  6. additionA 0.1 N solution of hydrochloric acid in isopropanol is then added
  7. customAfter evaporation under vacuum