反应详情

Dioxane (5 mL) was charged in a flask. 3-{4-[3-(7-Fluoro-quinolin-6-ylmethyl)-imidazo[1,2-b]pyridazin-6-yl]-pyrazol-1-yl}-azetidine-1-carboxylic acid tert-butyl ester (Stage 146.2, 100 mg, 0.200 mmol) and HCl in dioxane (4 M solution, 500 μL, 2.002 mmol) were then added and the mixture was stirred at rt for 1 h. The RM was diluted with EtOAc/NaHCO3. The organic layer was separated and washed with brine (2×) then dried over Na2SO4, filtered and concentrated. The residue was purified by flash chromatography (CombiFlash® Companion System®, with a 4 g RediSep® silica gel column, DCM/(DCM/MeOH 19:1)=100:0→0:100) and precipitated in Et2O to afford the title compound as a foam (tR 2.87 min (conditions 3), MH+=400.1).

1. customThe organic layer was separated
2. washwashed with brine (2×)
3. dry with materialthen dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by flash chromatography (CombiFlash® Companion System®
7. customwith a 4 g RediSep® silica gel column, DCM/(DCM/MeOH 19:1)=100:0→0:100) and precipitated in Et2O