Reaktion #2298615

Reaktionsgleichung

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

Ausbeute 96.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 1 hour
2. 2
   ExtraktionThe aqueous mixture was extracted with diethyl ether
3. 3
   WaschenThe organic layer was washed with water
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   Sonstigethe solvent evaporated under reduced pressure

Vorschrift

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.

Quelle