反应详情

温度

110 °C

To a solution of 33 (38 mg, 0.075 mmol) in freshly distilled DME (1 mL) was added 2,3-dihydropyrano[4,3,2-de]quinolin-7-ylboronic acid hydrochloride (24 mg, 0.097 mmol), chloro(2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl)[2-(2-aminoethylphenyl)]palladium(II) methyl-t-butylether adduct, [SPhos Palladacycle] (5 mg, 0.0075 mmol), and cesium fluoride (46 mg, 0.3 mmol). The reaction mixture was heated in the microwave at 110° C. for 45 min. A saturated solution of NaHCO3 (3 mL) was added, and the layers were separated. The aqueous layer was extracted with EtOAc. The combined organic layer were dried, filtered, and concentrated in vacuo. The crude material was purified by column chromatography (EtOAc/hexanes) to give 21 mg of 34. LCMS-ESI+: calc'd for C30H33N3O4S: 532.2 (M+H+); Found: 532.0 (M+H+).

1. customthe layers were separated
2. extractionThe aqueous layer was extracted with EtOAc
3. customThe combined organic layer were dried
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude material was purified by column chromatography (EtOAc/hexanes)