反应详情

温度

70 °C

To a two-neck round bottom flask with a magnetic stirring bar, was added tris(dibenzylideneacetone)dipalladium(0) (120 mg, 0.131 mmol), tri-t-butylphosphonium tetrafluoroborate (76 mg, 0.262 mmol), cesium fluoride (2.65 g, 17.5 mmol), 2,6-dimethylphenylboronic acid (1.3 g, 8.73 mmol), and the compound from Step A (1 g, 4.4 mmol). One neck of the flask was connected to a vacuum line while another neck was fitted with a argon balloon. The flask was then purged 8-10 times with argon. The vacuum line was replaced with a septum and anhydrous THF (10 mL) was added by syringe. The mixture was stirred in a 70° C. oil bath for 16 h. The reaction solution was filtrated and concentrated. The residue was purified by column chromatography on silica gel Biotage 40S™, eluting with EtOAc/hexane (10:1) to give the title compound as a clear oil.

1. customOne neck of the flask was connected to a vacuum line while another neck
2. customwas fitted with a argon balloon
3. customThe flask was then purged 8-10 times with argon
4. additionwas added by syringe
5. filtrationThe reaction solution was filtrated
6. concentrationconcentrated
7. customThe residue was purified by column chromatography on silica gel Biotage 40S™
8. washeluting with EtOAc/hexane (10:1)