反应详情

温度

80 °C

[5-(4-Bromo-phenyl)-3-methyl-isoxazol-4-yl]-carbamic acid 1-(2-chloro-phenyl)-ethyl ester (0.200 g, 0.46 mmol), 4-pentynoic acid (0.054 g, 0.55 mmol), copper iodide (spatula tip), triethylamine (0.12 mL, 0.84 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.053 g, 0.05 mmol) were combined in DME (5 mL), and the reaction was purged with N2 for 15 minutes and then stirred at 80° C. overnight. The mixture was partitioned between EtOAc and H2O, and the aqueous layer was separated and extracted with EtOAc. The combined organic layers were dried over MgSO4, filtered, and concentrated, and the residue was purified by preparative HPLC to give the title compound. Mass spec. data (M+H)=453.

1. customthe reaction was purged with N2 for 15 minutes
2. customThe mixture was partitioned between EtOAc and H2O
3. customthe aqueous layer was separated
4. extractionextracted with EtOAc
5. dry with materialThe combined organic layers were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customthe residue was purified by preparative HPLC