反应详情

温度

80 °C

3b (1.0 g, 2.4 mmol), benzophenone imine (0.4 mL, 2.4 mmol), sodium tert-butoxide (350 mg, 3.6 mmol), BINAP (150 mg, 0.27 mmol), and Pd2dba3 (55 mg, 0.06 mmol) were dissolved in toluene (10 mL) and degassed for 10 minutes with N2. The reaction was then sealed and heated to 80° C. for 2 hours. After cooling to room temperature, the reaction was diluted with EtOAc and brine, and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over MgSO4, filtered, and concentrated, and the residue was purified by silica gel chromatography (30% EtOAc in hexanes) to give the desired product, 3c.

1. customdegassed for 10 minutes with N2
2. customThe reaction was then sealed
3. temperatureAfter cooling to room temperature
4. additionthe reaction was diluted with EtOAc and brine
5. extractionthe aqueous layer was extracted with EtOAc
6. dry with materialThe combined organic layers were dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customthe residue was purified by silica gel chromatography (30% EtOAc in hexanes)