HRID1795166
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
- 100 °C
PROCEDURE
实验过程
To a solution of 4-cyclohexyl-4-methanesulfonyloxymethyl-piperidine-1-carboxylic acid tert-butyl ester, 4, (2.42 g, 6.73 mmol) in DMF (25 mL) is added sodium azide (1.32 g, 20.2 mmol) and the mixture is heated and stirred at 100° C. over night. The reaction is cooled and then quenched with water. The resulting solution is extracted with EtOAc (30 mL), dried, filtered and concentrated in vacuo to afford the crude product as a brown oil which is purified via chromatography on silica gel eluting with hexane/EtOAc 3:1 to afford the desired product in 76% yield (1.91 g) as a colorless oil.
WORKUP
后处理
- temperaturethe mixture is heated
- temperatureThe reaction is cooled
- customquenched with water
- extractionThe resulting solution is extracted with EtOAc (30 mL)
- customdried
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto afford the crude product as a brown oil which
- customis purified via chromatography on silica gel eluting with hexane/EtOAc 3:1