HRID656883
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
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
- customall the solvents were then removed
- dissolutionThe residues were redissolved in MeOH
- stirringstirred with amberlyst ion exchange resin until a neutral pH
- filtrationThe resin was filtered off
- customthe solvent removed
- customthe crude residues were purified by column chromatography on silica gel using a 0-20% 2M NH3