تفاعل #2298621
ord-867ac4ad339d4d5ba9c5951f2f52e8fb
معادلة التفاعل
7-bromo-3H-thieno[3,2-d]pyrimid-4-one
7-Bromo-3H-thieno[3,2-d]pyrimid-4-one
phosphorus oxychloride
sodium bicarbonate
→
7-bromo-4-chlorothieno[3,2-d]pyrimidine
المردود 82.0%
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةat reflux for 1 hour
- 2استخلاصThe aqueous mixture was extracted with ethyl acetate
- 3غسيلThe organic layer was washed with water
- 4تجفيفdried over anhydrous magnesium sulfate
- 5أخرىthe solvent evaporated under reduced pressure
الإجراء التجريبي
A solution of 7-bromo-3H-thieno[3,2-d]pyrimid-4-one (126, 0.94 g, 4.1 mmol) in phosphorus oxychloride (4 mL) under N2 was heated at reflux for 1 hour. The resulting solution was 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 ethyl acetate. 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 7-bromo-4-chlorothieno[3,2-d]pyrimidine (0.83 g, 82% yield) as a yellow solid.