HRID1659991

反应详情

EQUATION

反应方程式

HRID 1659991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

500 cm3 of acetone and a solution of 99 g of dimethylamine in 250 cm3 of acetone were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was cooled to 0° C. and then 139 g of 7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acid were introduced. The mixture was agitated at ambient temperature, the acetone distilled off and the residue dissolved in 1 liter of water. The solution was rendered alkaline, filtered and treated with 70 cm3 of hydrochloric acid. The precipitate was dried off, washed and dried. 128 g of 7-dimethylsulfamoyl-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 220°-221° C.; yield: 89%).

WORKUP

后处理

  1. customprovided with an agitator
  2. distillationthe acetone distilled off
  3. dissolutionthe residue dissolved in 1 liter of water
  4. filtrationfiltered
  5. additiontreated with 70 cm3 of hydrochloric acid
  6. customThe precipitate was dried off
  7. washwashed
  8. customdried