反应详情

A mixture of 3-(4-Bromo-3-methyl-phenyl)-5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazole (500 mg), 1,4-butandiol-monovinyl ether (385 mg), 1,3-bis(diphenylphosphine)propane (dppp, 9 mg), palladium on charcoal (10%, 23 mg), dicylohexylmethylamine (259 mg) and n-butanol (3 mL) were stirred under an atmosphere of nitrogen at reflux over night. After cooling, ethyl acetate (30 mL) and aqueous hydrochloric acid (1 M, 20 mL) were added and the mixture was stirred at room temperature for 1 h. After filtration, the layers were separated, the organic layer was extracted with 1 M HCl, dried (Na2SO4) and evaporated in vacuum. Purification of the residue on silica gel afforded the title compound (270 mg, 60%).

1. temperatureat reflux over night
2. temperatureAfter cooling
3. stirringthe mixture was stirred at room temperature for 1 h
4. filtrationAfter filtration
5. customthe layers were separated
6. extractionthe organic layer was extracted with 1 M HCl
7. dry with materialdried (Na2SO4)
8. customevaporated in vacuum
9. customPurification of the residue on silica gel