HRID656883

反应详情

EQUATION

反应方程式

HRID 656883 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1,1-Dimethylethyl (1-{2-[7-(methyloxy)-2-oxo-1(2H)-quinolinyl]ethyl}-4-piperidinyl)carbamate (2.25 g; 5.61 mmol) was dissolved in a mixture of chloroform (20 ml) and HCl (15 ml) and stirred at rt under argon for 1 hour. The salts were dissolved in MeOH and a small amount of toluene added, all the solvents were then removed. The residues were redissolved in MeOH and stirred with amberlyst ion exchange resin until a neutral pH was reached. The resin was filtered off and the solvent removed and the crude residues were purified by column chromatography on silica gel using a 0-20% 2M NH3:MeOH/DCM gradient, to give the desired product (900 mg; 54%).

WORKUP

后处理

  1. customall the solvents were then removed
  2. dissolutionThe residues were redissolved in MeOH
  3. stirringstirred with amberlyst ion exchange resin until a neutral pH
  4. filtrationThe resin was filtered off
  5. customthe solvent removed
  6. customthe crude residues were purified by column chromatography on silica gel using a 0-20% 2M NH3