反应详情

To a solution of 0.0282 g (0.15 mmol) 17 in 1 mL EtOAc was added 0.0034 g Pd (10% on C). After 5 h under H2 at atmospheric pressure, the reaction mixture was diluted with 30 mL EtOAc and filtered over celite. The celite was washed with 200 mL EtOAc, and the filtrate was concentrated in vacuo. Purification by flash chromatography (10×160 mm silica gel, 5% (10% NH40H:MeOH):CH2Cl2) yielded 18. 1H NMR (CDCl3, 400 MHz) δ 9.272 (s, 1H, ArH); 8.583 (d, 1H, J=5.94 Hz, ArH); 7.876 (dd, 2H, J=7.18, 11.57 Hz, ArH); 7.583 (t, 1H, J=7.64 Hz, ArH); MS (Electrospray): m/z 159.0 (M+H).

1. filtrationfiltered over celite
2. washThe celite was washed with 200 mL EtOAc
3. concentrationthe filtrate was concentrated in vacuo
4. customPurification by flash chromatography (10×160 mm silica gel, 5% (10% NH40H:MeOH):CH2Cl2)