反応 #2298615

反応方程式

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

収率 96.0%

反応条件

後処理

1. 1
   温度at reflux for 1 hour
2. 2
   抽出The aqueous mixture was extracted with diethyl ether
3. 3
   洗浄The organic layer was washed with water
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他the solvent evaporated under reduced pressure

実験手順

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.

出典