Reaktion #216221

Reaktionsgleichung

aminosulfonyl-6-isopropyl-4-methoxy-N,N-diethylbenzamide

→

4-isopropyl-6-methoxysaccharin

Ausbeute 91.0%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

A solution of 2.aminosulfonyl-6-isopropyl-4-methoxy-N,N-diethylbenzamide (429.6 g) in acetic acid (1.5 L) was refluxed for 20 hours, then cooled to room temperature. The solvent was removed under vacuum. The oily residue was dissolved in water (6 L) and the pH was adjusted to 1 with hydrochloric acid (6N). The crude product was collected by filtration, washed with water (2 L), dried at 60° C. under vacuum for 18 hours and recrystallized from ethyl acetate-hexane to give 4-isopropyl-6-methoxysaccharin (303 g, 91% yield, m.p. 188° C.).

Quelle