HRID1906528

反应详情

EQUATION

反应方程式

HRID 1906528 的结构方程式

PROCEDURE

实验过程

6.0 g of 2-(4-tert-butylphenyl)-7-hydroxy-6-nitro-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one was added to a mixture of 25 ml of phosphorus oxychloride and 4 ml of diethylaniline, and the resulting mixture was heated at a temperature of 70° to 80° C. for 2 hours. After cooling, the precipitate formed was filtered, washed successively with water, isopropanol and diethyl ether to obtain 4.3 g of 2-(4-tert-butylphenyl)-7-chloro-6-nitro-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-5-one as crystals having a melting point of 245° to 248° C.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated at a temperature of 70° to 80° C. for 2 hours
  2. temperatureAfter cooling
  3. customthe precipitate formed
  4. filtrationwas filtered
  5. washwashed successively with water, isopropanol and diethyl ether