HRID2075713
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
To 9b (29 mg, 0.07 mmol) in DMF (1 mL) was added sodium azide (9 mg, 0.09 mmol). The reaction was heated at 130° C. overnight, then cooled to room temperature and diluted with EtOAc and water. The aqueous layer was extracted with EtOAc, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The crude material was purified by silica gel chromatography (50% EtOAc in hexanes) to give the desired product, 9c.
WORKUP
后处理
- temperaturecooled to room temperature
- extractionThe aqueous layer was extracted with EtOAc
- dry with materialthe combined organic layers were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude material was purified by silica gel chromatography (50% EtOAc in hexanes)