反应详情

To a solution of 200 mg (0.50 mmol) 5-chloro-thiophene-2-carboxylic acid [2-(1-isopropyl-piperidin-4-ylsulfamoyl)-ethyl]-amide in 3 ml dichloromethane were added 0.1 ml (2 equiv.) 1-isocyanato-propane and 6 mg DMAP. The reaction mixture was stirred overnight at room temperature. The next day further 0.1 ml (2 equiv.) 1-isocyanato-propane and 6 mg DMAP were added. After stirring for 48 h at room temperature, the reaction mixture was washed with 3 ml water and concentrated under reduced pressure. Final purification by preparative RP-HPLC (CH3CN/H2O gradient+0.1% TFA) gave pure 5-chloro-thiophene-2-carboxylic acid {2-[(1-isopropyl-piperidin-4-yl)-propylaminocarbonyl-sulfamoyl]-ethyl}-amide. The title compound was obtained as its trifluoroacetate in form of a colorless amorphous material.

1. stirringAfter stirring for 48 h at room temperature
2. washthe reaction mixture was washed with 3 ml water
3. concentrationconcentrated under reduced pressure
4. customFinal purification by preparative RP-HPLC (CH3CN/H2O gradient+0.1% TFA)