Реакция #1687634
ord-dddecb71856e4b40b10c34c0a9991333
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ТемператураThe suspension was refluxed for 4 h
- 2Фильтрацияfiltered
- 3ДругоеThe toluene phase was separated
- 4Экстракцияthe aqueous phase extracted with 2×100 ml of toluene
- 5СушкаThe combined organic phase were dried over MgSO4
- 6Другоеevaporated in vacuo
- 7Другоеleaving a heavy, yellow oil, 88
Методика
To a solution of 8.0 g (0.045 mol) of 73 in 125 ml of toluene, 10 g (0.045 mol) of P4S10 was added. The suspension was refluxed for 4 h and left at room temperature overnight. The mixture was poured into ice water followed by basification with ammonia. The two-phase system was stirred with charcoal and filtered. The toluene phase was separated and the aqueous phase extracted with 2×100 ml of toluene. The combined organic phase were dried over MgSO4 and evaporated in vacuo leaving a heavy, yellow oil, 88. Yield: 2.3 g (0.013 mol), 29%).