Реакция #2298626
ord-34e2d7db353e435aa16e02584e3844b6
Уравнение реакции
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
Выход 81.0%
Реактанты
Реагенты
Нет
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураat reflux for 1 hour
- 2Экстракцияextracted with ethyl acetate
- 3ПромывкаThe organic layer was washed with water
- 4Сушкаdried over anhydrous magnesium sulfate
- 5Другоеthe solvent evaporated under reduced pressure
Методика
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.