Potassium Carbonate → HCID 19012068, compound

Participants

Reaction Steps

5 ml of a dichloromethane solution containing 0.65 ml of anhydrous trifluoromethanesulfonic acid was added at -78° C. to 25 ml of a dichloromethane solution containing 1.3 g of 6-[4-(3-[4-aminophenoxy]propyl)piperazin-1-yl]-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione obtained in Example 6, and the temperature of the solution was then gradually elevated to room temperature, while it was stirred. 20 ml of dichloromethane and a 2% aqueous potassium carbonate solution were added to the reaction solution, followed by stirring until insolubles were dissolved therein. After the separation of the resultant organic layer, the aqueous layer was neutralized and then extracted with chloroform (50 ml×2), and the extract layers were joined and mixed with the organic layer previously obtained. The mixture was dried over sodium sulfate and then concentrated to obtain 1.1 g (yield: 62.5%) of 6-[4-(3-[4-trifluoromethanesulfonylaminophenoxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione in a crystalline state.

Provenance & Evidence