HRID1612635

反应详情

EQUATION

反应方程式

HRID 1612635 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

100 g (0.51 mol) of 7-methoxycarbonylbenzo-1,2,3-thiadiazole are suspended in 1000 ml of water, and then 310 ml of 2N sodium hydroxide solution and 5 ml of dioxane are added. The reaction mixture is heated to 40° C., is stirred for 4 hours at that temperature and is then cooled to 10° C. A further 1000 ml of water are added and the batch is neutralised with 310 ml of 2N hydrochloric acid. The resulting precipitate is isolated by filtration, lightly dried in a current of air and then dissolved in tetrahydrofuran and the solution is dried over magnesium sulfate, filtered and concentrated. The crystals are suspended in hexane, isolated by filtration and dried.

WORKUP

后处理

  1. temperatureis then cooled to 10° C
  2. customThe resulting precipitate is isolated by filtration
  3. customlightly dried in a current of air
  4. dissolutiondissolved in tetrahydrofuran
  5. dry with materialthe solution is dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customisolated by filtration
  9. customdried