Реакция #11365
ord-1a9df976ff5240b3a21e1366d2833d10
Уравнение реакции
Реактанты
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураheated
- 2Температураat reflux for 2 h
- 3Экстракцияextraction with CH2Cl2
- 4Сушкаdrying over MgSO4 and concentration under reduced pressure
- 5Другоеthe residue was triturated with ether
- 6ДругоеThis gave 1.33 g (33% pure according to LC-MS) of the desired product which was reacted further without further purification
Методика
A solution, cooled to 0° C., of 1 g (3.1 mmol) of the compound from example 17A in 80 ml of CH2Cl2 was admixed dropwise with 1.2 g (6.1 mmol) of bromoacetyl bromide and a little at a time with 1.2 g (9.1 mmol) of AlCl3. The reaction mixture was warmed to room temperature (30 min.) and then heated at reflux for 2 h and carefully poured into ice-water. Following extraction with CH2Cl2, drying over MgSO4 and concentration under reduced pressure, the residue was triturated with ether. This gave 1.33 g (33% pure according to LC-MS) of the desired product which was reacted further without further purification.