تفاعل #2298615

معادلة التفاعل

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

المردود 96.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 1 hour
2. 2
   استخلاصThe aqueous mixture was extracted with diethyl ether
3. 3
   غسيلThe organic layer was washed with water
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   أخرىthe solvent evaporated under reduced pressure

الإجراء التجريبي

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.

المصدر