반응 #1675637

반응 방정식

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

용매

toluene

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도the resulting solution is refluxed for 24 hours
2. 2
   온도It is cooled
3. 3
   기타The organic phase is separated off
4. 4
   추출the water phase is extracted twice with dichloromethane
5. 5
   기타The organic phase is dried
6. 6
   기타evaporated
7. 7
   기타After 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
   기타are obtained

실험 절차

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.

출처