HRID924481

反应详情

EQUATION

反应方程式

HRID 924481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the tert-butyl [(3S,5R)-1-[3-({[3-amino-7-(1-methylpiperidin-4-yl)quinolin-2-yl]carbonyl}amino)pyridin-4-yl]-5-(trifluoromethyl)piperidin-3-yl]carbamate, 1 mL of 4 M HCl in dioxane and 1 mL of MeOH were added. The mixture was stirred at room temperature for 1 h, then evaporated under vacuum. The resulting residue was dissolved in 4.5 mL of MeOH and treated with 0.3 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 C27H33F3N7O [M+H]+: m/z=528.3. found: 528.3.

WORKUP

后处理

  1. customevaporated under vacuum
  2. dissolutionThe resulting residue was dissolved in 4.5 mL of MeOH
  3. additiontreated with 0.3 mL of NH4OH solution
  4. filtrationThe mixture was filtered
  5. customthe filtrate was purified by preparative HPLC (XBridge™ C18 column
  6. washeluting with a gradient of MeCN/water containing 0.1% NH4OH, at a flow rate of 30 mL/min.)