反应详情

温度

75 °C

To a solution of compound 13 (900 mg, 2.55 mmol) in MeOH (30 mL) was added Pd(OH)2/C (120 mg). The mixture was stirred at 75° C. under H2 (50 psi) overnight. The suspension was filtered through Celite, washed with MeOH (20 mL×2). The combined organic phases were concentrated in vacuo to afford compound 14 (540 mg, 80% yield) as a white solid. LC-MS: m/z 265 [M+H]+. 1H NMR (400 MHz, CDCl3): δ 9.07 (br. s, 1H), 7.85 (s, 1H), 4.84 (q, J=6.4 Hz, 1H), 4.11 (m, 2H), 3.59 (m, 2H), 3.44˜3.39 (m, 1H), 2.14˜2.06 (m, 3H), 1.92˜1.88 (m, 2H), 1.64 (d, J=6.4 Hz, 3H).

1. filtrationThe suspension was filtered through Celite
2. washwashed with MeOH (20 mL×2)
3. concentrationThe combined organic phases were concentrated in vacuo