HRID656938

反应详情

EQUATION

反应方程式

HRID 656938 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-(5,7-difluoro-2-oxo-1(2H)-quinolinyl)ethyl]-4-piperidinyl}carbamate (2 g; 4.9 mmol) was dissolved in chloroform (20 ml) and 4M HCl in 1,4-dioxane added (20 ml), this was stirred at rt for 1 h. The salts were then dissolved in MeOH and all solvents removed. The residues were redissolved in MeOH and stirred with amberlyst ion exchange resin until neutral pH was reached, the resin was filtered off and solvents removed. 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 (970 mg; 65%).

WORKUP

后处理

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