HRID918186

反应详情

EQUATION

反应方程式

HRID 918186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,4-disulfamoyl-6-bromoaniline (0.015 mole) and chloroacetyl chloride (0.016 mole) in 50 ml. of dioxane or other inert organic solvent is heated under reflux conditions for about 24 hours and then concentrated to dryness. The residue is dissolved in concentrated sulfuric acid (5 ml. acid/gram), heated in a steam bath at 60°-70° C. for three hours then poured onto ice. The product, 3-chloromethyl-5-bromo-7-sulfamoyl-1,2,4-benzothiadiazine-1,1-dioxide, is purified by recrystallization from a mixture of acetone-alcohol-water.

WORKUP

后处理

  1. concentrationconcentrated to dryness
  2. dissolutionThe residue is dissolved in concentrated sulfuric acid (5 ml. acid/gram)
  3. temperatureheated in a steam bath at 60°-70° C. for three hours
  4. additionthen poured onto ice
  5. customThe product, 3-chloromethyl-5-bromo-7-sulfamoyl-1,2,4-benzothiadiazine-1,1-dioxide, is purified by recrystallization from a mixture of acetone-alcohol-water