Reacción #2298615

Ecuación de reacción

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

Rendimiento 96.0%

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturaat reflux for 1 hour
2. 2
   ExtracciónThe aqueous mixture was extracted with diethyl ether
3. 3
   LavadoThe organic layer was washed with water
4. 4
   Secadodried over anhydrous magnesium sulfate
5. 5
   Otrothe solvent evaporated under reduced pressure

Procedimiento

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.

Fuente