反应详情

(4-[(Cyclopropylamino)carbonyl]-1-{4-[(ethylamino)carbonyl]phenyl}-1H-1,2,3-triazol-5-yl)methyl methanesulfonate (195 mg, 0.479 mmol) obtained in Example 126a), potassium carbonate (66.1 mg, 0.479 mmol, 1.0 eq.) and morpholine (0.085 ml, 0.957 mmol, 2.0 eq.) were suspended in acetonitrile (4.0 ml), and the mixture was stirred at room temperature for 15 hr. The reaction mixture was diluted with ethyl acetate (30 ml) and washed with 2% aqueous sodium carbonate solution, saturated aqueous sodium hydrogen carbonate solution and saturated brine. The aqueous layers were each extracted with ethyl acetate (15 ml). The organic layers were combined, dried over anhydrous sodium sulfate and concentrated. Diethyl ether was added and the precipitate was collected by filtration and crystallized from ethyl acetate. The precipitate was collected by filtration and crystallized from ethanol again to give the title compound as a white powder (142 mg, 0.356 mmol, 74.4%).

1. washwashed with 2% aqueous sodium carbonate solution, saturated aqueous sodium hydrogen carbonate solution and saturated brine
2. extractioneach extracted with ethyl acetate (15 ml)
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated
5. additionDiethyl ether was added
6. filtrationthe precipitate was collected by filtration
7. customcrystallized from ethyl acetate
8. filtrationThe precipitate was collected by filtration
9. customcrystallized from ethanol again