HRID649025

反应详情

EQUATION

反应方程式

HRID 649025 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6-cyano-2-dimethylaminothioxanthen-9-one 10,10-dioxide, 2.0 g (0.006 mol), ethylenediamine, 3 g, 0.05 mol, and sodium methoxide, 0.1 g (0.002 mol) in methanol, 30 ml, was refluxed for 48 hr. The mixture was poured into H2O and the resultant precipitate was dissolved in boiling in 1N HCl. This solution was cooled and the dihydrochloride salt was filtered and recrystallized from 95% ethanol to yield 2-dimethylamino-6-(2-imidazolin-2-yl)thioxanthen-9-one 10,10-dioxide dihydrochloride 0.3 g with m.p. 330°-335° C. (dec); TLC on silica gel (ethylacetate:ethanol:acetic acid/80:15:5), Rf =0.4.

WORKUP

后处理

  1. temperature30 ml, was refluxed for 48 hr
  2. temperatureThis solution was cooled
  3. filtrationthe dihydrochloride salt was filtered
  4. customrecrystallized from 95% ethanol