反应详情

Intermediate (27) (0.0128 mol), 1,4-dioxane (50 ml), and O-(trimethylsilyl)hydroxyl-amine, (0.134 mol) were combined under argon. The reaction mixture was stirred at RT for 20 hours. The reaction mixture was concentrated and DCM (50 ml), NaOH (1 N; 50 ml), and HCl (1N; 100 ml) were added. The solution was stirred for one hour. The precipitate was filtered off and recrystallized from methanol. The precipitate was filtered off and dried, yielding 2.96 g (59.8%) of 4-[[4-[(2,6-dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl] amino]benzonitrile monohydrochloride.monohydrate (compound 21).

1. concentrationThe reaction mixture was concentrated
2. additionDCM (50 ml), NaOH (1 N; 50 ml), and HCl (1N; 100 ml) were added
3. stirringThe solution was stirred for one hour
4. filtrationThe precipitate was filtered off
5. customrecrystallized from methanol
6. filtrationThe precipitate was filtered off
7. customdried