反应详情

A 10 mL, CEM microwave vessel was charged with 3 (0.1040 g, 0.427 mmol), 1-(5-phenylpyridin-2-yl)hydrazine (4, 0.119 g, 0.641 mmol), a stirbar and 1 mL concentrated HCl. The vessel was sealed, and fitted with an 18-guage needle and an Argon inlet. The slurry was placed in a heating block at 115° C. for 15 minutes with stirring. A volatile substance evolved during this time. The vessel was briefly cooled, and the seal was replaced. The vessel was irradiated on a CEM Explorer using the following parameters: ramp time 20 s, hold time 10 min, hold temperature 150° C., powermax=on, 75 W max. The resultant turbid aqueous solution was filtered and concentrated in vacuo. The solids were suspended in 3 mL hot EtOH, and cooled. The precipitate was isolated by filtration and washed with EtOH (3×3 mL). The solids were taken up in 2 mL H2O, and filtered through a 0.1 μm PVDF Ultra-free-CL centrifugal filter (Millipore Corp, PN UFC40W00, 2000 g for 5 minutes). The aqueous filtrate was lyophilized to afford 6-((6-phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)isoquinoline hydrochloride. Anal. Calcd for C21H15N5. HCl.1.7H2O: C, 62.36; H, 4.83; N, 17.31. Found: C, 62.39±0.08; H, 4.48±0.02; N, 17.28±0.03.

1. customThe vessel was sealed
2. customfitted with an 18-guage needle and an Argon inlet
3. temperatureThe vessel was briefly cooled
4. customThe vessel was irradiated on a CEM Explorer
5. customtime 20 s
6. customtime 10 min
7. customtemperature 150° C., powermax=
8. filtrationwas filtered
9. concentrationconcentrated in vacuo
10. temperaturecooled
11. customThe precipitate was isolated by filtration
12. washwashed with EtOH (3×3 mL)
13. filtrationfiltered through a 0.1 μm PVDF Ultra-free-CL centrifugal
14. filtrationfilter (Millipore Corp, PN UFC40W00, 2000 g for 5 minutes)