反应详情

Triethylamine (1.2 ml) was added at ambient temperature to a solution of 3-(4-bromo-3-methyl-phenyl)-5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazole (1.2 g) (Example I3) in ethanol (45 ml). Bis(triphenylphosphine)palladium(II) dichloride (“PdCl2(PPh3)2”) (0.185 g) was added and the reaction mixture was stirred in a pressure reactor in an atmosphere of carbon monoxide (120 bar) at 115° C. for 8 hours. The reaction mixture was cooled to ambient temperature, filtered over Celite® and concentrated. The residue was purified by preparative HPLC to give 4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzoic acid ethyl ester (0.85 g) as a yellow oil. 1H-NMR (CDCl3, 400 MHz): 7.95 (d, 1H), 7.55 (m, 4H), 7.45 (s, 1H), 4.40 (q, 2H), 4.10 (d, 1H), 3.7 (d, 1H), 2.60 (s, 3H), 1.40 (t, 3H) ppm.

1. filtrationfiltered over Celite®
2. concentrationconcentrated
3. customThe residue was purified by preparative HPLC