反应详情

A mixture of Example 42C (0.087 g, 0.27 mmol), and platinum oxide (0.056 g, 0.25 mmol) in acetic acid (7.5 mL) was shaken in a reactor pressurized with 60 psi of H2 at 25° C. for 80 hours and filtered. The filtrate was concentrated and the concentrate was purified by C18 reverse-phase HPLC with acetonitrile/water/0.1% trifluoroacetic acid to provide the desired-product. MS (ESI(+)) m/e 332 (M+H)+, 349 (M+NH4)+, 354 (M+Na)+; (ESI(−) m/e 330 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 7.74 (m, 2H), 7.63 (m, 1H), 7.56 (m, 2H), 6.98 (d, 1H), 6.63 (d, 1H), 2.65 (m, 4H), 1.66 (m, 4H).

1. filtrationfiltered
2. concentrationThe filtrate was concentrated
3. customthe concentrate was purified by C18 reverse-phase HPLC with acetonitrile/water/0.1% trifluoroacetic acid
4. customto provide the desired-product