HRID596867
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 solution of the hydrochloride (80 g) of methyl 2-(p-methoxybenzyl)-4-oxo-1,3,3-trimethyl-5-piperidinecarboxylate in 450 ml of 1 N hydrochloric acid is refluxed for 12 hours. After cooling, some resinous material is removed by extraction with ether. Alkalinization of the aqueus solution with the aid of ammonia causes the separation of the piperidone which is extracted with ether. Concentration in vacuo of the extent gives a residue which is dissolved in ethanolic hydrogen chloride. Evaporation of the ethanol leaves a syrupy residue which is dissolved in acetone, whereafter the crystalline hydrochloride separates. Yield 87%. Melting point 168° - 170° C, with decomposition.
WORKUP
后处理
- temperatureAfter cooling
- customsome resinous material is removed by extraction with ether
- customthe separation of the piperidone which
- extractionis extracted with ether
- concentrationConcentration in vacuo of the extent
- customgives a residue which
- customEvaporation of the ethanol
- customleaves a syrupy residue which