反应详情

5-Nitroindazole (3.44 g, 21.08 mmol) was suspended in N,N-dimethylformamide (100 ml) and sodium hydride (0.93 g, 23.19 mmol) was slowly added to the suspension at 0° C., followed by stirring for 30 min and then for an additional 30 min at room temperature. The addition of 1-((2-(2,4-difluorophenyl)oxiran-2-yl)methyl)-1H-1,2,4-triazole (5 g, 21.08 mmol) was performed before stirring at 60° C. for 2 hours. The addition of water (1 ml) at 0° C. led to termination of the reaction. After being diluted with ethyl acetate (200 ml), the reaction mixture was washed with saturated ammonium chloride solution (200 ml) and then with brine (200 ml). The organic layer was dried over anhydrous magnesium sulfate and vacuum evaporated to concentrate it. The product was purified by chromatography on silica gel to give the title compound (Yield 47%). This compound was found to have a melting point from 63 to 64° C.

1. waitfor an additional 30 min at room temperature
2. stirringbefore stirring at 60° C. for 2 hours
3. customled to termination of the reaction
4. washthe reaction mixture was washed with saturated ammonium chloride solution (200 ml)
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate and vacuum
6. customevaporated
7. concentrationto concentrate it
8. customThe product was purified by chromatography on silica gel