反应详情

温度

95 °C

The 1-(2,4-difluorophenyl)-2-(3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone (0.20 g, 0.63 mmol, Preparation #K.1), N,N-dimethylformamide dimethyl acetal (0.14 g, 1.14 mmol) and toluene (2 mL) were heated in an about 110° C. oil bath. After about 30 min, the mixture was cooled and the solvent was concentrated under reduced pressure. The residue was dissolved in 1,4-dioxane (2 mL) and hydrazine (0.0360 mL, 1.14 mmol) was added. The mixture was heated to about 95° C. in an oil bath for about 30 min, cooled to ambient temperature, and then concentrated under reduced pressure. The material was purified by RP-HPLC (Table 1, Method d). Concentration of the desired fractions under reduced pressure resulted in precipitation of a tan solid that was collected by filtration and then dried to give the title compound (0.054 g, 25%): LC/MS (Table 1, Method a) Rt=1.69 min; MS m/z: 341.2 (M+H)+.

1. temperaturethe mixture was cooled
2. concentrationthe solvent was concentrated under reduced pressure
3. dissolutionThe residue was dissolved in 1,4-dioxane (2 mL)
4. temperaturecooled to ambient temperature
5. concentrationconcentrated under reduced pressure
6. customThe material was purified by RP-HPLC (Table 1, Method d)
7. customConcentration of the desired fractions under reduced pressure resulted in precipitation of a tan solid
8. filtrationthat was collected by filtration
9. customdried