反应 #2298615

反应方程式

7-methyl-3H-thieno[3,2-d]pyrimid-4-one

7-Methyl-3H-thieno[3,2-d]pyrimid-4-one

phosphorus oxychloride

sodium bicarbonate

→

4-chloro-7-methylthieno[3,2-d]pyrimidine

收率 96.0%

反应条件

后处理

1. 1
   温度at reflux for 1 hour
2. 2
   萃取The aqueous mixture was extracted with diethyl ether
3. 3
   洗涤The organic layer was washed with water
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   其他the solvent evaporated under reduced pressure

实验过程

A solution of 7-methyl-3H-thieno[3,2-d]pyrimid-4-one (3, 2.9 g, 18 mmol) in phosphorus oxychloride (18 mL) under N2 was heated at reflux for 1 hour. The resulting solution as allowed to cool to room temperature and then poured into a saturated aqueous solution of sodium bicarbonate to neutralize. The aqueous mixture was extracted with diethyl ether. The organic layer was washed with water followed by saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and the solvent evaporated under reduced pressure to yield 4-chloro-7-methylthieno[3,2-d]pyrimidine (3.1 g, 96% yield) as a white solid.

来源