HRID1154724

反应详情

EQUATION

反应方程式

HRID 1154724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionTo a suspension of 1.8 g
  2. temperatureThe reaction mixture is heated
  3. temperatureto reflux
  4. temperatureheating
  5. filtrationAt this time the reaction mixture is filtered
  6. customto remove insoluble material
  7. customevaporated to dryness
  8. customThe product is purified
  9. customThe desired fraction was evaporated to dryness
  10. customtriturated with ether
  11. customto give 120 mg