反应详情

温度

60 °C

To a cooled (0° C.) suspension of NaH (55% mineral oil dispersion, 288 mg, 6.6 mmol, washed with hexane) in DMF (25 mL) was added 1,2,4-triazole (0.5 g, 7.2 mmol) and the mixture was stirred at 0° C. until hydrogen gas ceased to evolve. Then, a solution of unpurified (2R,3S)-3-(2,4-difluorophenyl)-3,4-epoxy-2-methylbutanoic acid (0.5 g) (obtained in reference example 29) in DMF (3 mL) was slowly added and the mixture was heated to 60° C. during 2 h. A saturated NH4Cl aqueous solution was then added and the solvents were removed in vacuo. The mixture was then partitioned between brine containing AcOH and EtOAc. The organic layer was separated and the aqueous phase was extracted with more EtOAc (3×). The collected organic fractions were then dried over anhydrous Na2SO4, the drying agent was filtered and the flitrate was concentrated under reduced pressure to a white solid. Recrystallization from EtOAc afforded the title product as a white solid.

1. temperatureTo a cooled
2. customthe solvents were removed in vacuo
3. customThe mixture was then partitioned between brine
4. additioncontaining AcOH and EtOAc
5. customThe organic layer was separated
6. extractionthe aqueous phase was extracted with more EtOAc (3×)
7. dry with materialThe collected organic fractions were then dried over anhydrous Na2SO4
8. filtrationthe drying agent was filtered
9. concentrationthe flitrate was concentrated under reduced pressure to a white solid
10. customRecrystallization from EtOAc