HRID223362

反应详情

EQUATION

反应方程式

HRID 223362 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5.8 g (0.02 mole) 5-chloro-4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 2.0 g (0.02 mole) triethylamine, and 100 ml ether was added 2.2 g (0.02 mole) ethyl chloroformate. An immediate reaction ensued and a precipitate formed. After refluxing 2 hours longer the mixture was filtered, and the filtrate was washed with aqueous potassium carbonate and then with water. Rotary evaporation yielded 5.4 g residue which was recrystallized from ligroin to give 4.6 g (69% yield) of pure product (mp 43.5°-44.5° C.). The structure was confirmed via infrared and elemental analysis.

WORKUP

后处理

  1. customAn immediate reaction
  2. customa precipitate formed
  3. temperatureAfter refluxing 2 hours longer the mixture
  4. filtrationwas filtered
  5. washthe filtrate was washed with aqueous potassium carbonate
  6. customRotary evaporation