反应详情

To 2.53 g of N-[3-(1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]acetamide in 100 ml of dry dimethylformamide was added 0.6 g of sodium hydride (50% in oil). This mixture was stirred under argon, for 1 hour, then 0.78 ml of methyl iodide was added. This mixture was stirred overnight, then poured into 300 ml of water and extracted with 50 ml portions of dichloromethane. The extracts were combined, dried and evaporated in vacuo. The residue was chromatographed on a silica gel column, eluting with dichloromethane:methanol (98:2). The active fractions were combined, evaporated and the solid recrystallized from dichloromethane-hexane, giving 1.39 g of the desired product as light orange crystals mp 166°-169° C.

1. stirringThis mixture was stirred overnight
2. extractionextracted with 50 ml portions of dichloromethane
3. customdried
4. customevaporated in vacuo
5. customThe residue was chromatographed on a silica gel column
6. washeluting with dichloromethane:methanol (98:2)
7. customevaporated
8. customthe solid recrystallized from dichloromethane-hexane