反应详情

温度

85 °C

2,2-Bis(5-chloro-pyrid-2-yl)oxirane (0.8 g), 1,2,4-triazole (1.0 g) and anhydrous potassium carbonate (3.0 g) were stirred in dry N,N-dimethylformamide (30 ml) and the mixture was heated at 85° C. for 1.5 hours. The solvent was then evaporated under vacuum, with the addition of xylene to remove final traces of N,N-dimethylformamide as an azeotrope, and the residue was dissolved in water (20 ml) and extracted with ethyl acetate (3×20 ml). The combined organic extracts were dried over megnesium sulfate and evaporated. The residue was chromatographed on silica, eluting with ethyl acetate. Evaporation of the relevant fractions gave a viscous oil which solidified on trituration with petroleum ether (b.p. 60°-80° C.). Recrystallization from hexane gave the title compound as white crystals (0.48 g, 38%) m.p. 98°-100° C.

1. customThe solvent was then evaporated under vacuum, with the addition of xylene
2. customto remove final traces of N,N-dimethylformamide as an azeotrope
3. dissolutionthe residue was dissolved in water (20 ml)
4. extractionextracted with ethyl acetate (3×20 ml)
5. dry with materialThe combined organic extracts were dried over megnesium sulfate
6. customevaporated
7. customThe residue was chromatographed on silica
8. washeluting with ethyl acetate
9. customEvaporation of the relevant fractions
10. customgave a viscous oil which
11. customRecrystallization from hexane