Реакция #2298615

Уравнение реакции

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

Выход 96.0%

Условия реакции

Обработка

1. 1
   Температураat reflux for 1 hour
2. 2
   ЭкстракцияThe aqueous mixture was extracted with diethyl ether
3. 3
   ПромывкаThe organic layer was washed with water
4. 4
   Сушкаdried over anhydrous magnesium sulfate
5. 5
   Другоеthe solvent evaporated under reduced pressure

Методика

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.

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