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 1-ethoxycarbonyl-4-diphenylmethoxypiperidine (60 g; 0.176 moles) and 85% potassium hydroxide (116 g; 1.76 moles) in isopropanol (600 ml) was boiled under reflux for 6 hours. After cooling, concentrated hydrochloric acid was added until pH=2 and the solvent removed in vacuo. The resulting residue was dissolved in a small quantity of water, washed with diethyl ether and the aqueous solution was made alkaline with aqueous sodium hydroxide solution and extracted with methylene chloride. The organic solution was dried (Na2SO4), the solvent removed in vacuo and the residual oil treated with ethanolic hydrogen chloride solution. 4-Diphenylmethoxy-piperidine hydrochloride (38 g; yield 71%) was obtained.
WORKUP
后处理
- temperatureunder reflux for 6 hours
- temperatureAfter cooling
- customthe solvent removed in vacuo
- dissolutionThe resulting residue was dissolved in a small quantity of water
- washwashed with diethyl ether
- extractionextracted with methylene chloride
- dry with materialThe organic solution was dried (Na2SO4)
- customthe solvent removed in vacuo
- additionthe residual oil treated with ethanolic hydrogen chloride solution