反应详情

温度

90 °C

A suspension of potassium trans-1-propenyltrifluoroborate (9.86 g, 66.7 mmol), PdCl2(dppf).DCM adduct (907 mg, 1.11 mmol), ethyl 5-bromo-4-methylisoxazole-3-carboxylate (Intermediate A) (13 g) and triethylamine (7.7 mL) in EtOH (250 mL) was degassed under vacuum and back-filled with nitrogen before heating at 90° C. for 18 h. After cooling to room temperature, the reaction was partitioned between EtOAc and brine, separated, dried over MgSO4 and concentrated under reduced pressure. The crude material was adsorbed onto silica and purification by chromatography eluting with 5-10% EtOAc in iso-hexane afforded the title compound;

1. additionback-filled with nitrogen
2. temperatureAfter cooling to room temperature
3. customthe reaction was partitioned between EtOAc and brine
4. customseparated
5. dry with materialdried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe crude material was adsorbed onto silica and purification by chromatography
8. washeluting with 5-10% EtOAc in iso-hexane