反应详情

温度

70 °C

6-Methyl-4-oxo-4H-chromene-2-carboxylic acid (Aldrich, 3.5 g, 17.1 mmol) was added to a mixture of acetic acid (50 mL) and 10% palladium on carbon (0.35 g) in a Parr shaker. The glass reactor was sealed and flushed with nitrogen, and pressurized with hydrogen (60 psi). The mixture was shaken at 70° C. for 2.5 hours, and filtered and solids were rinsed with methanol. The filtrate was concentrated under reduced pressure to afford the title compound. 1H NMR (300 MHz, CDCl3) δ ppm 2.09-2.23 (m, 1H), 2.25 (s, 3H), 2.28-2.40 (m, 1H), 2.72-2.86 (m, 2H), 4.71 (dd, J=8.48, 3.39 Hz, 1H), 6.83 (t, J=8.65 Hz, 2H), 6.90-6.96 (m, 1H). MS (ESI) m/z 210.1 (M+NH4)+.

1. customThe glass reactor was sealed
2. customflushed with nitrogen
3. filtrationfiltered
4. washsolids were rinsed with methanol
5. concentrationThe filtrate was concentrated under reduced pressure