HRID1581013
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
24 g. of 1-(4'-chloro benzyl)-2-phenyl-4-(β-hydroxy ethyl) piperazine are dissolved in 150 cc. of chloroform and added drop by drop to a solution of 15 g. of thionyl chloride in 150 cc. of chloroform. The mixture is boiled under reflux for 5 hours and the solvent is removed in a vacuum by heating the mixture in a water bath. Excess of absolute ethanolic hydrochloric acid is added and the remaining acid is distilled off. The crystalline residue obtained is recrystallized from absolute ethanol. Melting point 178°-195° C. (dec.); yield 30 g.
WORKUP
后处理
- temperatureunder reflux for 5 hours
- customthe solvent is removed in a vacuum
- temperatureby heating the mixture in a water bath
- additionExcess of absolute ethanolic hydrochloric acid is added
- distillationthe remaining acid is distilled off
- customThe crystalline residue obtained
- customis recrystallized from absolute ethanol