反应详情

温度

70 °C

To a stirred solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)4-iodo-3-methylpyrazole (2.06 g) in dimethylformamide (25 ml) was added tetrakis(triphenylphosphine)palladium(0) (0.1 g) and vinyltri-n-butyltin (2 ml). The mixture was heated at 70° C. for 2 hours. The reaction mixture was eyaporated and then partitioned between water and ether. The aqueous layer was separated and extracted twice with ether. The combined organic layers were washed with brine, dried (Na2SO4) and evaporated. The residue was purified by column chromatigraphy on silica gel eluted with hexane: ether (9:1). Combination and evaporation of appropriate fractions gave a yellow solid which was further purified by reverse phase high performance chromatography on C18 silica eluted with acetonitrile: methanol: water (40:10:50). Combination and evaporation of appropriate fractions gave the title compound as a white solid, m.p.68.1-68.7° C.

1. custompartitioned between water and ether
2. customThe aqueous layer was separated
3. extractionextracted twice with ether
4. washThe combined organic layers were washed with brine
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customThe residue was purified by column chromatigraphy on silica gel
8. washeluted with hexane: ether (9:1)
9. customCombination and evaporation of appropriate fractions
10. customgave a yellow solid which
11. customwas further purified by reverse phase high performance chromatography on C18 silica
12. washeluted with acetonitrile: methanol: water (40:10:50)
13. customCombination and evaporation of appropriate fractions