HRID1591756

反应详情

EQUATION

反应方程式

HRID 1591756 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 137 mg (0.29 mmol) of 2,3-dichloro-N-(2-{3-[2-(4-cyanophenyl)ethyl]-2-oxoimidazolidin-1-yl}ethyl)-N-methylbenzenesulphonamide, 2 ml of ethylenediamine and 4.6 mg (0.14 mmol) of sulphur was stirred at 100° C. for two hours. Water was then added, and the mixture was extracted with ethyl acetate. The organic extracts were washed with saturated sodium chloride solution, dried over sodium sulphate and concentrated. The crude product obtained in this manner was purified by column chromatography on silica gel (mobile phase: dichloromethane/methanol/NH3 13:1:0.1 to 8:1:0.1). Using etheral hydrochloric acid, the product was then converted into the hydrochloride and freeze-dried.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic extracts were washed with saturated sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated