Reaktion #1675637

Reaktionsgleichung

trimethylaluminum

1-pyrrolidinosulfonylethanesulfonamide

methyl 4-methoxy-6-methyl-1,3,5-triazin-2-ylcarbamate

→

3-(4-Methoxy-6-methyl-1,3,5-triazin-2-yl)-1-(1-pyrrolidinosulfonylethylsulfonyl)urea

Lösungsmittel

toluene

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe resulting solution is refluxed for 24 hours
2. 2
   TemperaturIt is cooled
3. 3
   SonstigeThe organic phase is separated off
4. 4
   Extraktionthe water phase is extracted twice with dichloromethane
5. 5
   SonstigeThe organic phase is dried
6. 6
   Sonstigeevaporated
7. 7
   SonstigeAfter the crude product has been triturated with diethyl ether, 2.9 g (47% of theory) of 3-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-1-(1-pyrrolidinosulfonylethylsulfonyl)urea of melting point 136°-137° C.
8. 8
   Sonstigeare obtained

Vorschrift

9 ml (0.018 mol) of a 2M solution of trimethylaluminum in toluene are added dropwise at room temperature to 3.6 g (0.015 mol) of 1-pyrrolidinosulfonylethanesulfonamide (Example 1a) in 150 ml of dichloromethane. When the evolution of gas has ceased, 3.6 g (0.018 mol) of methyl 4-methoxy-6-methyl-1,3,5-triazin-2-ylcarbamate in 30 ml of dichloromethane are added dropwise, and the resulting solution is refluxed for 24 hours. It is cooled and poured into 150 ml of ice-cold 1N hydrochloric acid. The organic phase is separated off, and the water phase is extracted twice with dichloromethane. The organic phase is dried and evaporated. After the crude product has been triturated with diethyl ether, 2.9 g (47% of theory) of 3-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-1-(1-pyrrolidinosulfonylethylsulfonyl)urea of melting point 136°-137° C. are obtained.

Quelle