反応 #1675637

反応方程式

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

溶媒

toluene

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   温度the resulting solution is refluxed for 24 hours
2. 2
   温度It is cooled
3. 3
   その他The organic phase is separated off
4. 4
   抽出the water phase is extracted twice with dichloromethane
5. 5
   その他The organic phase is dried
6. 6
   その他evaporated
7. 7
   その他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.
8. 8
   その他are obtained

実験手順

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.

出典