反应详情

温度

80 °C

In a 10 mL sealed tube under N2 were dissolved dichlorobis(triphenylphosphine)palladium (41 mg, 59 μmol), NAN-dimethylprop-2-yn-1-amine (97 mg, 1170 μmol), 4-((6-chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methoxy)-7-methoxyquinoline (prepared according to General Method A) (200 mg, 585 μmol), TRIETHYLAMINE (1631 μl, 11704 μmol) and COPPER(I) IODIDE (11 mg, 59 μmol) in 3 mL of MeCN then stirred and heated at 80° C. for 10 h. The crude reaction mixture was directly purified by MPLC (ISCO) with DCM/DCM:MeOH:NH4OH (90:10:1) 95:5 to afforded 3-(3-((7-methoxyquinolin-4-yloxy)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)-N,N-dimethylprop-2-yn-1-amine (26 mg, 11% yield) as a yellow solid. MS m/z=388.2[M+1]+. Calc'd for C21H20N6O2: 389.2.

1. customIn a 10 mL sealed tube under N2
2. customThe crude reaction mixture
3. customwas directly purified by MPLC (ISCO) with DCM/DCM