反应详情

N-Methyl piperazine (5 ml) and sulfamide (11.26 g) in 1,4-dioxane (100 ml) were heated at reflux for 48 h. The solvent was evaporated under reduced pressure and the resulting solid dissolved in a mixture of methanol and water and applied to a plug of SCX-silica followed by further elution with aqueous methanol. This was then followed by elution with 1M ammonia in methanol (×4) and these fractions collected and solvent evaporated to dryness leaving a white solid. This was triturated with Et2O and filtered leaving the subtitle compound as a white solid. Yield: 5.0 g.

1. temperatureat reflux for 48 h
2. customThe solvent was evaporated under reduced pressure
3. dissolutionthe resulting solid dissolved in a mixture of methanol and water
4. washfollowed by further elution with aqueous methanol
5. washThis was then followed by elution with 1M ammonia in methanol (×4)
6. customthese fractions collected
7. customsolvent evaporated to dryness
8. customleaving a white solid
9. customThis was triturated with Et2O
10. filtrationfiltered