反应详情

温度

0 °C

A mixture of 2-methyl-1-(3-nitro-pyrazol-1-yl)-propan-2-ol (1.31 g, 7.07 mmol), and DMF (60 mL) was stirred at 0° C. for 5 min, then NaH (60% dispersion in oil, 0.85 g, 21.2 mmol) was added and stirred 20 min at 0° C. R-(−)-glycidyl-3-nitrobenzenesulfonate (2.75 g, 10.6 mmol) was added and stirred at 0° C. for 1 h then warmed to rt for 14 h. The mixture was then diluted with NH4Cl(s), ethyl acetate, the organic phase was separated, washed with NaHCO3(satd) dried with Na2SO4, and filtered. The mixture was then concentrated and purified by column chromatography (40-240 g Analogix column, 70% EtoAc/heptane to yield the product 1-[2-methyl-2-((R)-1-oxiranylmethoxy)-propyl]-3-nitro-1H-pyrazole as a white solid (0.7 g, 41%).

1. stirringstirred 20 min at 0° C
2. stirringstirred at 0° C. for 1 h
3. temperaturethen warmed to rt for 14 h
4. customthe organic phase was separated
5. washwashed with NaHCO3(satd)
6. dry with materialdried with Na2SO4
7. filtrationfiltered
8. concentrationThe mixture was then concentrated
9. custompurified by column chromatography (40-240 g Analogix column, 70% EtoAc/heptane