反应详情

A mixture of benzyl [2-{[(4-{(3S,5R)-3-[(tert-butoxycarbonyl)amino]-5-methylpiperidin-1-yl}pyridin-3-yl)amino]carbonyl}-7-(4-methylpiperazin-1-yl)quinolin-3-yl]carbamate (0.006 g, 0.008 mmol) and 2 mL of 4.0 M HBr in AcOH was stirred at room temperature for 2 h. The solution was then concentrated under reduced pressure and the resulting residue was treated with 4.5 mL of MeOH and 0.5 mL of NH4OH solution. The mixture was filtered and purified by preparative HPLC (XBridge™ C18 column, eluting with a gradient of MeCN/water containing 0.1% NH4OH, at a flow rate of 30 mL/min.) to afford the title compound. LCMS calc. for C26H35N8O [M+H]+: m/z=475.3. found: 475.3.

1. concentrationThe solution was then concentrated under reduced pressure
2. additionthe resulting residue was treated with 4.5 mL of MeOH and 0.5 mL of NH4OH solution
3. filtrationThe mixture was filtered
4. custompurified by preparative HPLC (XBridge™ C18 column
5. washeluting with a gradient of MeCN/water containing 0.1% NH4OH, at a flow rate of 30 mL/min.)