反应详情

To a solution of (2RS,3RS)-2-(2,4-difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol (0.060 g), 4-bromomethyl-5-methyl-2-oxo-1,3dioxol (0.049 g) in N,N-dimethylformamide (2.0 ml) was added anhydrous potassium carbonate (0.20 g) at -20° C. and the mixture was stirred for 10 minutes. To the reaction mixture were added ethyl acetate (10 ml) and water (10 ml), and organic layer was separated. The mixture was further extracted with ethyl acetate (10 ml×2). The organic layers were combined, washed with saturated aqueous sodium chloride solution (10 ml), dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography (1 cm×5 cm), and elution was carried out with ethyl acetate-hexane (1:1). The desired fraction was concentrated and the residue was crystallized from chloroform-diethyl ether to give (2RS,3RS)-2-(2,4-difluorophenyl)-3-(5-methyl-2-oxo-1,3-dioxol-4-yl)methylthio-1-(1H-1,2,4-triazol-1-yl)-2-butanol (compound 56, 0.065 g). m.p. 173°-174° C.

1. customwas separated
2. extractionThe mixture was further extracted with ethyl acetate (10 ml×2)
3. washwashed with saturated aqueous sodium chloride solution (10 ml)
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. washThe residue was subjected to silica gel chromatography (1 cm×5 cm), and elution
7. concentrationThe desired fraction was concentrated
8. customthe residue was crystallized from chloroform-diethyl ether