HRID1995382

反应详情

EQUATION

反应方程式

HRID 1995382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 5 gm of 3-amino-4-methoxy-1,2-benzoisothiazole-1,1-dioxide and 1.63 gm of potassium cyanide in 15 ml of dimethyl-sulfoxide was heated to 130°-140° C. (bath temperature 160° C.) and kept at this temperature for 1.5 hours. After cooling, the reaction mixture was stirred into 250 ml of methylene chloride, and the resulting precipitate was filtered off, dried and dissolved in 30 ml of water. At 60° C. the solution was treated with charcoal and filtered while hot. The hot filtrate was adjusted to pH 1 with concentrated aqueous hydrochloric acid. After cooling, the resulting crystals were suction-filtered off, washed with a little ice water and dried in vacuo.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe resulting precipitate was filtered off
  3. customdried
  4. dissolutiondissolved in 30 ml of water
  5. additionAt 60° C. the solution was treated with charcoal
  6. filtrationfiltered while hot
  7. temperatureAfter cooling
  8. filtrationthe resulting crystals were suction-filtered off
  9. washwashed with a little ice water
  10. customdried in vacuo