Reaktion #1005369

Reaktionsgleichung

2,4-disulfamoyl-5-bromoaniline

chloroacetyl chloride

→

3-Chloromethyl-6-bromo-7-sulfamoyl-1,2,4-benzothiadiazine-1,1-dioxide

Lösungsmittel

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for about 24 hours
2. 2
   Einengenconcentrated to dryness
3. 3
   workup.DISSOLUTIONThe residue is dissolved in ethanol
4. 4
   Temperaturheated on the steam bath in a mixture of 2.0 g
5. 5
   TemperaturThe solution is cooled
6. 6
   Sonstigethe product separated by acidification with hydrochloric acid
7. 7
   Sonstigepurified by recrystallization from a mixture of ethanol and water

Vorschrift

A mixture of 2,4-disulfamoyl-5-bromoaniline (0.02 mole) and chloroacetyl chloride (0.022 mole) in 75 ml. of dioxane is heated under reflux for about 24 hours and then concentrated to dryness. The residue is dissolved in ethanol and then heated on the steam bath in a mixture of 2.0 g. of potassium or sodium acetate and 50 ml. of water for two hours. The solution is cooled and the product separated by acidification with hydrochloric acid and purified by recrystallization from a mixture of ethanol and water.

Quelle