反应详情

温度

100 °C

A 48-mL sealed tube equipped with a magnetic stirring bar was charged with bromide 101c (120 mg, 0.4 mmol), aniline 101g (168 mg, 0.4 mmol), diisopropyethylamine (0.08 mL, 0.48 mmol) in EtOH (3 mL). After the mixture was stirred at 100° C. for 16 h, aqueous Na2CO3 (5 mL) was added. The aqueous phase was extracted with EtOAc (2×5 mL), and the combined organic extracts were washed with brine (5 mL), dried with Na2SO4 and concentrated. The residue was chromatographed with (gradient, 50%-100% EtOAc/hexanes) to afford 100 mg (42%) of 101h.

1. customA 48-mL sealed tube
2. customequipped with a magnetic stirring bar
3. extractionThe aqueous phase was extracted with EtOAc (2×5 mL)
4. washthe combined organic extracts were washed with brine (5 mL)
5. dry with materialdried with Na2SO4
6. concentrationconcentrated
7. customThe residue was chromatographed with (gradient, 50%-100% EtOAc/hexanes)
8. customto afford 100 mg (42%) of 101h.