反应详情

温度

140 °C

A suspension of potassium trifluoro(vinyl)borate (241 mg, 1.800 mmol), 4-bromo-N-(2,4-dimethylphenyl)-N-isobutylbenzenesulfonamide (595 mg, 1.5 mmol), cesium carbonate (1466 mg, 4.50 mmol), palladium(II) chloride (5.32 mg, 0.030 mmol) and triphenylphosphine (23.61 mg, 0.090 mmol) was prepared in tetrahydrofuran (THF) (2 mL) and Water (0.2 mL). The mixture was heated to 140° C. by microwaves for 30 min, to yield a black suspension. Additional ½ eq of potassium trifluoro(vinyl)borate (121 mg, 0.9 mmol) was added, along with extra water (0.2 mL) and THF (2 mL) and reaction heated for a further 1 hour at 140° C. The reaction mixture was diluted with dichloromethane (15 mL) and water (5 mL), then filtered through a plug of celite to remove palladium catalyst. The resulting yellow solution was dried using a hydrophobic frit, concentrated, then purified by flash (Si) using 0-25% ethyl acetate/cyclohexane over 40 minutes. Fractions were combined to give a clear oil, 385.3 mg, and the product taken directly to the next step, without further purification. LCMS (M+1) 344, RT 1.48 mins.

1. customto yield a black suspension
2. temperatureheated for a further 1 hour at 140° C
3. filtrationfiltered through a plug of celite
4. customto remove palladium catalyst
5. customThe resulting yellow solution was dried
6. concentrationconcentrated
7. custompurified by flash (Si)
8. customover 40 minutes
9. customto give a clear oil, 385.3 mg
10. customthe product taken directly to the next step, without further purification
11. customLCMS (M+1) 344, RT 1.48 mins