反应详情

To a 20 mL microwave tube was added 5-bromo-2-tetralone (2.0 g, 8.9 mmol) and Palladium(0) Tetrakis (0.616 g, 0.533 mmol), zinc cyanide (1.0 g, 8.9 mmol), and DMF (8 mL). The tube was sealed, degassed and microwaved at 80° C. for 1.0 hour. TLC showed no starting material left. The mixture was diluted with ethyl acetate, washed with ammonium hydroxide (2M, 2×), dried with sodium sulfate, filtered and evaporated under reduced pressure. The product was purified by silica gel chromatography with isocrartic 30% ethyl acetate-hexane to furnish the title compound. 1H-NMR (500 MHz, CDCl3) δ ppm 7.57 (s, 1H), 7.55 (d, J=7.8 Hz, 1H), 7.28 (d, J=7.8 Hz, 1H), 3.67 (s, 2H), 3.14 (t, J=7.0 Hz, 2H), 2.60 (t, J=7.0 Hz, 2H).

1. customThe tube was sealed
2. customdegassed
3. custommicrowaved at 80° C. for 1.0 hour
4. waitleft
5. additionThe mixture was diluted with ethyl acetate
6. washwashed with ammonium hydroxide (2M, 2×)
7. dry with materialdried with sodium sulfate
8. filtrationfiltered
9. customevaporated under reduced pressure
10. customThe product was purified by silica gel chromatography with isocrartic 30% ethyl acetate-hexane