HRID1154724
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
To a suspension of 1.8 g. (0.0082 m.) of 3-(methylthio)thieno[3,4-d]isothiazole-1,1-dioxide in 10 ml. of ethanol is added 1.76 g. (0.0082 m.) of 2-[[[5-[(dimethylamino)methyl]-2-furanyl]methyl]thio]ethylamine with stirring at room temperature. The reaction mixture is heated to reflux and heating is continued for 1.5 hours. At this time the reaction mixture is filtered to remove insoluble material and then evaporated to dryness. The product is purified using a silica gel column with methanol as the eluant. The desired fraction was evaporated to dryness and then triturated with ether to give 120 mg. a white solid with a m.p. 100°-103° C.
WORKUP
后处理
- additionTo a suspension of 1.8 g
- temperatureThe reaction mixture is heated
- temperatureto reflux
- temperatureheating
- filtrationAt this time the reaction mixture is filtered
- customto remove insoluble material
- customevaporated to dryness
- customThe product is purified
- customThe desired fraction was evaporated to dryness
- customtriturated with ether
- customto give 120 mg