反应详情

2-(2-Fluoro-4-trifluoromethylphenyl)-2-(1,2,4-triazole-1-ylmethyl)oxirane (0.4 g.) and 3-(4-fluorophenyl)-1,2,4-triazole (0.3 g.) were added to a solution of sodium hydride (0.1 g. of a 50% dispersion in oil) in tert-butyl alcohol (10 ml.) and the mixture was heated at 80° for 16 hours. The reaction mixture was evaporated to dryness and the residual gum was partitioned between ethyl acetate and water. The organic layer was separated, dried and evaporated to dryness. The residual gum was chromatographed on a K60 silica column, eluting successively with chloroform/petroleum ether (b.p. 60°-80° C.) 60/40 v/v, 70/30 v/v and 80/20 v/v, to give 2-[3-(4-fluorophenyl)-1,2,4-triazole-1-yl]-1-(2-fluoro-4-trifluoromethylphenyl)-1-(1,2,4-triazole-1-ylmethyl)-ethanol, m.p. 96°-100°.

1. customThe reaction mixture was evaporated to dryness
2. customthe residual gum was partitioned between ethyl acetate and water
3. customThe organic layer was separated
4. customdried
5. customevaporated to dryness
6. customThe residual gum was chromatographed on a K60 silica column
7. washeluting successively with chloroform/petroleum ether (b.p. 60°-80° C.) 60/40 v/v, 70/30 v/v and 80/20 v/v