反应详情

A mixture of 2.0 g of -N-methyl-3-(3-methyl-1,2,4-triazolo-[4,3-b]pyridazin-6-yl)benzenamine and 2.14 ml of diketene in 250 ml of dry toluene was heated to reflux for 2 days. The solution was concentrated in vacuo and the residue partitioned between 300 ml dichloromethane and 200 ml of water. The aqueous layer was extracted with 150 ml portions of dichloromethane. The organic layer and extracts were combined, dried and concentrated in vacuo. The residue was chromatographed on 300 g of silica gel with dichloromethane-methanol (97:3). The fractions containing product were combined, evaporated in vacuo and the solid recrystalized from dichloromethane-hexane to give 1.15 g of tan crystals, mp 138°-141° C.

1. temperaturewas heated
2. temperatureto reflux for 2 days
3. concentrationThe solution was concentrated in vacuo
4. customthe residue partitioned between 300 ml dichloromethane and 200 ml of water
5. extractionThe aqueous layer was extracted with 150 ml portions of dichloromethane
6. customdried
7. concentrationconcentrated in vacuo
8. customThe residue was chromatographed on 300 g of silica gel with dichloromethane-methanol (97:3)
9. additionThe fractions containing product
10. customevaporated in vacuo
11. customthe solid recrystalized from dichloromethane-hexane