Reaktion #216218

Reaktionsgleichung

2-aminosulfonyl-6-isopropyl-N,N-diethylbenzamide

→

4-isopropylsaccharin

Ausbeute 90.0%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was removed under vacuum
2. 2
   workup.DISSOLUTIONThe oily residue was dissolved in water (500 mL)
3. 3
   FiltrationThe crude product was collected by filtration
4. 4
   Waschenwashed with water (300 mL)
5. 5
   Sonstigedried at 60° C. under vacuum for 18 hours
6. 6
   Sonstigerecrystallized from ether-hexane

Vorschrift

A solution of 2-aminosulfonyl-6-isopropyl-N,N-diethylbenzamide (60 g) in acetic acid (400 mL) was refluxed for 24 hours, then cooled to room temperature. The solvent was removed under vacuum. The oily residue was dissolved in water (500 mL) and the pH was adjusted to 1 with hydrochloric acid (2N). The crude product was collected by filtration, washed with water (300 mL), dried at 60° C. under vacuum for 18 hours and recrystallized from ether-hexane to give 4-isopropylsaccharin (40 g, 90% yield, m.p. 177° C.).

Quelle