반응 #2298615

반응 방정식

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

수율 96.0%

반응 조건

후처리

1. 1
   온도at reflux for 1 hour
2. 2
   추출The aqueous mixture was extracted with diethyl ether
3. 3
   세척The organic layer was washed with water
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   기타the solvent evaporated under reduced pressure

실험 절차

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.

출처