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
3.4 g of 1-(4-aminobenzoyl)-4-[2-(4-chlorophenyl)ethyl]piperazine and 2.6 g of 2-isopropyloxyethyl p-toluenesulfonate are suspended in 30 ml of toluene and heated to boiling point. The clear solution so obtained is boiled under reflux for 17 hours and then concentrated by evaporation. Water is added to the residue, and the mixture is rendered alkaline with concentrated sodium hydroxide solution and extracted by shaking with methylene chloride. The crude oil is chromatographed over silica gel and crystallised in the form of the hydrochloride from acetone, yielding 1-{4-[N-(2-isopropyloxyethyl)amino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine hydrochloride having a melting point of 184°-185°.
WORKUP
后处理
- temperatureheated
- customThe clear solution so obtained
- temperatureunder reflux for 17 hours
- concentrationconcentrated by evaporation
- additionWater is added to the residue
- extractionextracted
- customThe crude oil is chromatographed over silica gel
- customcrystallised in the form of the hydrochloride from acetone