HRID903137

反应详情

EQUATION

反应方程式

HRID 903137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-amino-6-chloro-1,3-benzenedisulfonamide (5.72 g., 0.02 mole) and 4-dimethylaminocyclohexanone (3.38 g., 0.022 mole) in 2 N ethanolic HCl (100 ml) is refluxed for one hour and cooled. 4'-Dimethylamino-6-chlorospiro[2H-1,2,4-benzothiadiazine-3(4H),1'-cyclohexane]-7-sulfonamide-1,1-dioxide hydrochloride is filtered, dissolved in warm water (200 ml.) and treated with aqueous ammonia (1.0 ml.) to give 4'-dimethylamino-6-chlorospiro[2H-1,2,4-benzothiadiazine-3(4H),1'-cyclohexane]-7-sulfonamide-1,1-dioxide which melts at 255° C. after recrystallization from dimethylsulfoxide--H2O.

WORKUP

后处理

  1. temperatureis refluxed for one hour
  2. temperaturecooled
  3. filtration4'-Dimethylamino-6-chlorospiro[2H-1,2,4-benzothiadiazine-3(4H),1'-cyclohexane]-7-sulfonamide-1,1-dioxide hydrochloride is filtered
  4. dissolutiondissolved in warm water (200 ml.)
  5. additiontreated with aqueous ammonia (1.0 ml.)