HRID2092306

反应详情

EQUATION

反应方程式

HRID 2092306 的结构方程式

PROCEDURE

实验过程

To a round-bottomed flask were added methanol (70 ml, 91 mmol), glacial acetic acid (70 ml, 1212 mmol), and 7-methylquinazolin-4(3H)-one (14.56 g, 91 mmol). The reaction mixture was stirred at room temperature for 5 min followed by the slow addition of bromine (9.3 ml, 182 mmol). The reaction was stirred at room temperature for 3 h. Volatiles were evaporated under reduced pressure and the resulting crude residue washed with aqueous sodium thiosulfate to remove excess bromine and HBr, then oven dried to afford 6-bromo-7-methylquinazolin-4(3H)-one as light yellow amorphous solid. MS (M+H)+ 239, 241.

WORKUP

后处理

  1. stirringThe reaction was stirred at room temperature for 3 h
  2. customVolatiles were evaporated under reduced pressure
  3. washthe resulting crude residue washed with aqueous sodium thiosulfate
  4. customto remove excess bromine and HBr
  5. customoven dried