反应详情

温度

70 °C

tert-butyl 2-(4-bromo-5-oxo-2,5-dihydrofuran-3-yl)-1-oxo-2,8-diazaspiro[4.5]decane-8-carboxylate (2.2 g, 5.30 mmol), potassium trifluoro(vinyl)borate (1.06 g, 7.95 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (0.345 g, 0.530 mmol) and potassium phosphate tribasic (10.60 mL, 10.60 mmol) were taken up in THF (44.1 mL) in a sealed tube, de-gassed and the resulting mixture was heated overnight at 70° C. The reaction mixture was cooled to room temperature and then was diluted with EtOAc and water. After separation of layers, the aqueous layer was extracted with EtOAc (2×). The combined organic layers were dried over anhydrous MgSO4, filtered, concentrated and purified by silica gel column chromatography using (30-100) % EtOAc/hexanes as mobile phase to provide the title compound.

1. customde-gassed
2. temperatureThe reaction mixture was cooled to room temperature
3. additionwas diluted with EtOAc and water
4. customAfter separation of layers
5. extractionthe aqueous layer was extracted with EtOAc (2×)
6. dry with materialThe combined organic layers were dried over anhydrous MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. custompurified by silica gel column chromatography