反应详情

A solution of Example 186A (17 mg, 0.03 mmol) in 2 mL of ethanol was degassed, treated with palladium on carbon (˜1 mg, 10%), put under an atmosphere of hydrogen, stirred for 4 h at room temp, filtered through a plug of celite, and concentrated to afford a yellow solid. The crude material was chromatographed on silica gel with a gradient of methanol in dichloromethane (0-10%) to afford the title compound (8.2 mg, 51% yield). 1H NMR (300 MHz, DMSO-d6) δ ppm 0.44 (m, 1H) 0.70 (s, 9H) 0.79 (m, 1H) 1.39 (s, 3H) 1.74 (m, J=3.31 Hz, 1H) 2.15 (td, J=12.41, 4.23 Hz, 1H) 4.12 (s, 2H) 7.22 (s, 1H) 7.33 (m, 1H) 7.48 (m, 2H) 8.04 (d, J=7.35 Hz, 1H) 8.17 (br. s, 2H) 16.99 (s, 1H); MS (APCI+) m/z 474 (M+H)+.

1. filtrationfiltered through a plug of celite
2. concentrationconcentrated
3. customto afford a yellow solid
4. customThe crude material was chromatographed on silica gel with a gradient of methanol in dichloromethane (0-10%)