HRID1731410

反应详情

EQUATION

反应方程式

HRID 1731410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 0.9 g. (0.0044 mole) of thieno[3,4-d]isothiazole-3(2H)-thione 1,1-dioxide in 4 ml. of ethanol is added a solution of 0.35 g. (0.0044 mole) of 50% sodium hydroxide in 3 ml. of water. To this thick mixture is added 0.62 g. (0.0044 mole) of iodomethane. The mixture is heated under reflux for 5 minutes, and then filtered to give 0.35 g. of product. On cooling, a second crop of 0.1 g. of material is obtained. A small amount of the first crop is recrystallized from ethanol to afford an analytical sample, m.p. 184°-6° C.

WORKUP

后处理

  1. additionTo a mixture of 0.9 g
  2. additionTo this thick mixture is added 0.62 g
  3. temperatureThe mixture is heated
  4. temperatureunder reflux for 5 minutes
  5. filtrationfiltered
  6. customto give 0.35 g
  7. temperatureOn cooling
  8. customof material is obtained
  9. customA small amount of the first crop is recrystallized from ethanol
  10. customto afford an analytical sample, m.p. 184°-6° C.