HRID649025
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 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
- temperature30 ml, was refluxed for 48 hr
- temperatureThis solution was cooled
- filtrationthe dihydrochloride salt was filtered
- customrecrystallized from 95% ethanol