HRID924484
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of benzyl [2-{[(4-{(3S,5R)-3-[(tert-butoxycarbonyl)amino]-5-methylpiperidin-1-yl}pyridin-3-yl)amino]carbonyl}-7-(2-oxopiperidin-1-yl)quinolin-3-yl]carbamate (0.005 g, 0.007 mmol) in 2 mL of 33% HBr in AcOH was stirred at room temperature for 2 h. The mixture was evaporated to dryness under reduced pressure. The resulting residue was dissolved in 4 mL of MeOH and treated with 0.5 mL of NH4OH solution. The mixture was filtered and the filtrate was 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 C26H32N7O2 [M+H]: m/z=474.3. found: 474.6.
WORKUP
后处理
- customThe mixture was evaporated to dryness under reduced pressure
- dissolutionThe resulting residue was dissolved in 4 mL of MeOH
- additiontreated with 0.5 mL of NH4OH solution
- filtrationThe mixture was filtered
- customthe filtrate was purified by preparative HPLC (XBridge™ C18 column
- washeluting with a gradient of MeCN/water containing 0.1% NH4OH, at a flow rate of 30 mL/min.)