HRID66718

反应详情

EQUATION

反应方程式

HRID 66718 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 5.7 g (0.025 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 2.6 g (0.025 mole) triethylamine, and 100 ml acetonitrile was added 5.8 g (0.025 mole) diphenylcarbamoyl chloride. The reaction mixture was refluxed 4 hours. A precipitate was filtered out and ether was added to the filtrate yielding more precipitate. Rotary evaporation gave 9.3 g residue which was recrystallized from ligroin to give 6.15 g (58% yield) of product. An analytical sample was recrystallized a second time from ligroin and had mp 132°-134° C. The structure was confirmed via infrared and elemental analysis.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed 4 hours
  2. filtrationA precipitate was filtered out and ether
  3. additionwas added to the filtrate
  4. customyielding more precipitate
  5. customRotary evaporation