HRID470616
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
A mixture of 4-oxo-piperidine-1-carboxylic acid tert-butyl ester (compound of Example 13; 13.5 g, 67 mmol), anhydrous potassium carbonate (11.22 g, 81 mmol) and cyanomethyl phosphonic acid diethylester (15.6 g, 88 mmol) in THF (70 mL) was heated at reflux for 12 h. THF was evaporated and the residue was dissolved in chloroform (2×50 mL). The resulting solution was washed with water (2×50 mL) and brine (50 mL). The organic phase obtained was dried over anhydrous sodium sulphate and concentrated to afford the title compound.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for 12 h
- customTHF was evaporated
- dissolutionthe residue was dissolved in chloroform (2×50 mL)
- washThe resulting solution was washed with water (2×50 mL) and brine (50 mL)
- customThe organic phase obtained
- dry with materialwas dried over anhydrous sodium sulphate
- concentrationconcentrated