HRID2041525
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
PROCEDURE
实验过程
Add 4N hydrogen chloride in dioxane (10 mL) to a solution of 3-tert-butoxycarbonylaminomethyl-6-cyclohexylmethyl-pyridine (345 mg, 1.13 mmol) in EtOAc (10 mL) and stir overnight. Concentrate in vacuo, suspend the solid obtained in diethyl ether and add hexane. Filter and wash the solid with hexane. Suspend the solid into dichloromethane, add saturated aqueous NaHCO3 and stir until both phases are clear (15 min). Extract the aqueous phase twice with dichoromethane. Dry the combined organic extracts over MgSO4, filter and concentrate in vacuo to obtain the title compound as an oil (205 mg, 97%) that was used without any further purification. MS (ES+) n7/z: 205 (M+H)+.
WORKUP
后处理
- concentrationConcentrate in vacuo
- customobtained in diethyl ether
- filtrationFilter
- washwash the solid with hexane
- additionadd saturated aqueous NaHCO3
- stirringstir until both phases
- custom(15 min)
- extractionExtract the aqueous phase twice with dichoromethane
- dry with materialDry the combined organic extracts over MgSO4
- filtrationfilter
- concentrationconcentrate in vacuo