反应详情

To a soluton of 1.9 g of 3-methyl-6-[3-(amino)phenyl]-1,2,4-triazolo[4,3-b]pyridazine and 1.6 of diisopropylethylamine in dichloromethane was added 1.67 g of trichloromethyl chloroformate. This mixture was stirred for 1 hour, then two equivalents of dimethylamine hydrochloride were added. Diisopropylethylamine was added until solution was complete then the mixture was stirred for 1 hour, poured into saturated aqueous sodium bicarbonate and extracted with dichloromethane. The extracts were combined, dried and the solvent removed. The residue was chromatographed on a 200 g silica gel column using dichloromethane:methanol (95:5) as eluent. The active fractions were combined, evaporated and the solid recrystallized from dichloromethane-methanol-hexane, giving 1.33 g of the desired product as pale yellow crystals, mp 237°-239° C.

1. stirringthe mixture was stirred for 1 hour
2. extractionextracted with dichloromethane
3. customdried
4. customthe solvent removed
5. customThe residue was chromatographed on a 200 g silica gel column
6. customevaporated
7. customthe solid recrystallized from dichloromethane-methanol-hexane