تفاعل #2298626
ord-34e2d7db353e435aa16e02584e3844b6
معادلة التفاعل
6-(3-thienyl)-3H-thieno[3,2-d]pyrimid-4-one
6-(3-Thienyl)-3H-thieno[3,2-d]pyrimid-4-one
phosphorus oxychloride
sodium bicarbonate
→
6-(3-thienyl)-4-chlorothieno[3,2-d]pyrimidine
المردود 81.0%
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةat reflux for 1 hour
- 2استخلاصextracted 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 6-(3-thienyl)-3H-thieno[3,2-d]pyrimid-4-one (218, 74 mg, 0.32 mmol) in phosphorus oxychloride (2 mL) under N2 was heated at reflux for 1 hour. The resulting solution was allowed to cool to room temperature, poured into a saturated aqueous solution of sodium bicarbonate to neutralize and then 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 6-(3-thienyl)-4-chlorothieno[3,2-d]pyrimidine (65 mg, 81% yield) as a yellow solid.