反应详情

To a mixture of ethyl 3-(2-Fluoro-6-iodo-phenyl)-5-methyl-isoxazole-4-carboxylate (0.25 g, 0.67 mmol), tetrakis(triphenylphosphine)palladium (0.08 g, 0.067 mmol), and Et3N (5 mL) under N2 was added TMSCN and heated at reflux overnight. The reaction was cooled to room temperature, diluted with H2O, and extracted with EtOAc (2×). The combined extracts were washed (H2O then brine), dried (MgSO4), filtered, and concentrated. Flash chromatography (silica gel, EtOAc/hexanes gradient) gave the title compound (0.15 g, 82%). Mass Spectrum (ES+) (m/z) 275.0 [M+1].

1. temperatureheated
2. temperatureat reflux overnight
3. extractionextracted with EtOAc (2×)
4. washThe combined extracts were washed (H2O
5. dry with materialbrine), dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated