反应详情

A mixture of (2R,3S)-2-(2,4-difluorophenyl)-3-methyl-2-(1H-1,2,4-triazol-1-yl)methyloxirane (1.0 g, 4.0 mmol), piperazine (860 mg, 10 mmol) and lithium perchlorate (625 mg, 6 mmol) in acetonitrile (15 ml) was heated under reflux for 48 h. The solvent was removed under reduced pressure, the residue was treated with crushed ice and extracted with ethylacetate (3×30 ml). The combined organic extract was washed with water, brine, dried (Na2SO4) and concentrated to give the title compound as thick viscous gum (1.5 g, 78%). The title compound was also prepared by hydrolysis of 2R,3R-2-(2,4-difluorophenyl)-3-(4-ethoxycarbonylpiperazin-1-yl)-1-(1H-1,2,4-triazol-1-yl)butan-2-ol 1 with 2M sodium hydroxide solution.

1. temperaturewas heated
2. temperatureunder reflux for 48 h
3. customThe solvent was removed under reduced pressure
4. additionthe residue was treated with crushed ice
5. extractionextracted with ethylacetate (3×30 ml)
6. extractionThe combined organic extract
7. washwas washed with water, brine
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated