HRID746911
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
Ethyl-1-benzyl-3-methyl-4-oxo-piperidine-3-carboxylate (85 g, 0.31 mol) was dissolved in conc HCl (82 ml, 0.77 mol) and the reaction mixture was heated to 100° C. for 32 hrs. Solvent was removed under reduced pressure and the resulting solid was dissolved in the 300 ml CHCl3 and 400 ml pet ether was added to this under stirring to provide a solid. The solid was filter and was dissolved in 400 ml ethyl acetate and organic layer was washed with 10% NaOH aqueous solution. Layers were separated and concentration of organic layer afforded 48 g (75%) oil as a titled product.
WORKUP
后处理
- customSolvent was removed under reduced pressure
- dissolutionthe resulting solid was dissolved in the 300 ml CHCl3 and 400 ml pet ether
- additionwas added to
- customto provide a solid
- filtrationThe solid was filter
- dissolutionwas dissolved in 400 ml ethyl acetate
- washorganic layer was washed with 10% NaOH aqueous solution
- customLayers were separated