HRID1190988
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
Dissolve (E)-3-(tert-butoxycarbonylamino-methyl)-6-(2-cyclohexylvinyl)-pyridine (1.3 g, 4.11 mmol) in EtOAc (60 mL) and bubble hydrogen chloride through the solution for 20 min. Stir the mixture overnight at room temperature. Concentrate the mixture in vacuo and dissolve the resulting solid in water. Adjust the pH to 9-11 with 20% aqueous K2CO3 and extract with DCM. Dry the combined organic extracts over MgSO4, filter and concentrate in vacuo to obtain the title compound (0.78 g, 88%). MS (APCI+) m/z: 217 (M+H)+.
WORKUP
后处理
- custombubble hydrogen chloride through the solution for 20 min
- concentrationConcentrate the mixture in vacuo
- dissolutiondissolve the resulting solid in water
- extractionextract with DCM
- dry with materialDry the combined organic extracts over MgSO4
- filtrationfilter
- concentrationconcentrate in vacuo