反应详情

温度

80 °C

To an ice cooled suspension of anhydrous K2CO3 (0.691 g, 0.005 mole) in N,N-dimethylformamide (7 ml), 1H-1,2,4-triazole (0.345, 0.005 mole) was added in small portions under art atmosphere of nitrogen. The mixture was slowly brought to room temperature and a solution of compound 7c (2R, 3S)-3-(2,4-Difluorophenyl)-3,4-epoxy-2-butanol (0.5 g, 0.0025 mole) in N,N-dimethylformamide (1 ml) was added. The resulting mixture was heated at 80° C. for 2 hours. The solvent was removed under reduced pressure and 25 g of crushed ice was added to the residue. The so formed mixture was extracted with ethyl acetate (50 ml, 2×25 ml). The combined organic layers were washed with water (10 ml) brine (25 ml) and dried over MgSO4. The solvent was removed in vacuo and the residue was chromatographed on silica gel. Elution with methanol in chloroform (0% -3%) gave the title compound 9c as an amorphous solid (0.26 g, 38%).

1. additionwas added in small portions under art atmosphere of nitrogen
2. customwas slowly brought to room temperature
3. customThe solvent was removed under reduced pressure and 25 g of crushed ice
4. additionwas added to the residue
5. customThe so formed mixture
6. extractionwas extracted with ethyl acetate (50 ml, 2×25 ml)
7. washThe combined organic layers were washed with water (10 ml) brine (25 ml)
8. dry with materialdried over MgSO4
9. customThe solvent was removed in vacuo
10. customthe residue was chromatographed on silica gel
11. washElution with methanol in chloroform (0% -3%)