HRID1263214

反应详情

EQUATION

反应方程式

HRID 1263214 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 6-ethoxy-2-benzothiazolesulfonamide (20 g.) and aluminum chloride (40 g.) in heptane (500 ml) was heated at reflux for 4 hours and cooled. The heptane was decanted from the reaction mixture which was then treated with ice water (500 ml.). After 1/2 hour the crude product was filtered, dissolved in warm dilute sodium hydroxide, filtered and acidified with concentrated hydrochloric acid to give 7.5 g of 6-hydroxy-2-benzothiazolesulfonamide which melts at 225°-228° C. after recrystallization from acetic acid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 4 hours
  3. temperaturecooled
  4. customThe heptane was decanted from the reaction mixture which
  5. additionwas then treated with ice water (500 ml.)
  6. filtrationAfter 1/2 hour the crude product was filtered
  7. dissolutiondissolved
  8. temperaturein warm dilute sodium hydroxide
  9. filtrationfiltered