反应详情

温度

65 °C

The compound from Example 1 (85 mg, 0.25 mmol) was dissolved in methanol (2 mL) followed by addition of 1N NaOH aqueous solution (0.27 ml, 0.27 mmol). The reaction solution was stirred at 60-70° C. for 4 h and then evaporated under vacuum to dryness. The residue was stirred with ethyl acetate (2 mL) and the solid was collected by filtration and washed with ethyl acetate to give the title product as an off-white solid (78 mg, 89.9%): MS (ESI) m/z 325 (M+1); 1H NMR (400 MHz, DMSO-d6) δ 1.99 (m, 2H), 2.45-2.51 (m, 6H), 3.01 (t, J=4.8 Hz, 4H), 6.67 (m, 1H), 6.88 (m, 4H), 6.98 (d, J=9.2 Hz, 2H), 7.13 (m, 2H), 7.75 (s, 1H).

1. customevaporated under vacuum to dryness
2. stirringThe residue was stirred with ethyl acetate (2 mL)
3. filtrationthe solid was collected by filtration
4. washwashed with ethyl acetate