HRID924452

反应详情

EQUATION

反应方程式

HRID 924452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of benzyl {2-[({4-[(3S,5R)-3-amino-5-methylpiperidin-1-yl]pyridin-3-yl}amino)carbonyl]-7-morpholin-4-ylquinolin-3-yl}carbamate (0.002 g, 0.003 mmol) in 2 mL of 4 M HBr in AcOH solution was stirred at room temperature for 2 h. The solution was then concentrated under reduced pressure and the residue was treated with 4.5 mL of MeOH and 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 C25H32N7O2 [M+H]+: m/z=462.3. found: 462.3.

WORKUP

后处理

  1. concentrationThe solution was then concentrated under reduced pressure
  2. additionthe residue was treated with 4.5 mL of MeOH and 0.5 mL of NH4OH solution
  3. filtrationThe mixture was filtered
  4. customthe filtrate was purified 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.)