Reaktion #214593

Reaktionsgleichung

1-ethyl-2-aminomethylpyrrolidine

chloroform

7-methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride

→

N-(1-ethyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide

Ausbeute 66.1%

Lösungsmittel

water chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONwas distilled
2. 2
   Filtrationthe remaining solution was filtered
3. 3
   SonstigeThe base was precipitated by the addition of 60 cm3 of 20% ammonia
4. 4
   SonstigeThe crystals formed
5. 5
   Sonstigewere dried off
6. 6
   Waschenwashed with water
7. 7
   Sonstigedried

Vorschrift

82 g of dextrorotatory 1-ethyl-2-aminomethylpyrrolidine, 600 ccm of chloroform and, gradually, at a temperature of from 5°-10° C., 200 g of 7-methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride were introduced into a balloon flask with an agitator and a thermometer. After the addition of a liter of water chloroform was distilled and then the remaining solution was filtered. The base was precipitated by the addition of 60 cm3 of 20% ammonia. The crystals formed were dried off, washed with water and then dried. 162 g of dextrorotatory N-(1-ethyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 136°-137° C.; yield: 66%).

Quelle