反应详情

A mixture 1.57 g of N-[3-(3-methyl-1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]cyclopropanecarboxamide, 0.36 g of sodium hydride (50% in oil) and 200 ml of dry dimethylformamide under argon was stirred at room temperature for 1 hour and then 0.60 ml of ethyl iodide was added. After stirring overnight, the mixture was poured into 200 ml of water and extracted with dichloromethane. The combined extracts were dried, the solvent removed and the residue chromatographed on a silica gel column with dichloromethane-methanol (97:3) as solvent. The fractions containing product were combined, the solvent removed and the solid recrystallized from dichloromethane-hexane to give 0.80 g of pale yellow crystals, mp 149°-151° C.

1. extractionextracted with dichloromethane
2. customThe combined extracts were dried
3. customthe solvent removed
4. customthe residue chromatographed on a silica gel column with dichloromethane-methanol (97:3) as solvent
5. additionThe fractions containing product
6. customthe solvent removed
7. customthe solid recrystallized from dichloromethane-hexane