反应详情

A mixture of Example 153 (185 mg, 0.53 mmol) and 10% Pd/C (37 mg) in MeOH (10 mL) was stirred under hydrogen (60 psi) for 16 h. The catalyst was removed by filtration through Celite, and the filtrate was concentrated to dryness. The residue was purified by flash chromatography on silica gel to give the desired product (107 mg, 72%). 1H NMR (300 MHz, DMSO-D6) δ ppm 0.95 (t, J=7.1 Hz, 6H) 1.73–1.82 (m, 2H) 2.29 (s, 3H) 2.41–2.50 (m, 6H) 2.68–2.73 (m, 2H) 5.25 (s, 2H) 6.80 (d, J=7.5 Hz, 1H) 7.17 (t, J=7.8 Hz, 1H) 7.25 (d, J=8.5 Hz, 1H) 7.31 (s, 1H) 7.36 (d, J=8.5 Hz, 2H) 7.43 (s, 1H) 7.59 (d, J=8.5 Hz, 2H) 7.68 (s, 1H) 8.66 (s, 1H) 8.85 (s, 1H) MS (ESI(+)) m/e 488.1 (M+H)+.

1. customThe catalyst was removed by filtration through Celite
2. concentrationthe filtrate was concentrated to dryness
3. customThe residue was purified by flash chromatography on silica gel