Реакция #64891
ord-b5cecb5335044841b71ce88453132533
Уравнение реакции
Реактанты
Реагенты
Растворители
Условия реакции
Температура
85°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ФильтрацияThe reaction mixture is filtered after 30 minutes
- 2Концентрированиеconcentrated in vacuo
- 3workup.ADDITIONThe residue is then diluted with water
- 4Экстракцияextracted with CH2Cl2
- 5СушкаThe extract is dried with Na2SO4
- 6Фильтрацияfiltered
- 7Концентрированиеconcentrated in vacuo
- 8ДругоеThe residue is then purified via flash chromatography (MeOH/CH2Cl2)
Методика
Zinc dust (1.3 g, 20 mmol) is added to a solution of the crude product from step A in 20 mL glacial acetic acid maintained at 85° C. The reaction mixture is filtered after 30 minutes and concentrated in vacuo. The residue is then diluted with water, basified with a 1.0N aqueous NaOH solution, and extracted with CH2Cl2. The extract is dried with Na2SO4, filtered and concentrated in vacuo. The residue is then purified via flash chromatography (MeOH/CH2Cl2) to provide the title compound.