反应详情

温度

0 °C

A solution of compound 23 (100 mg, 0.26 mmole) was dissolved in absolute ethanol (13 mL) and stirred at 0° C. for 10 minutes. A 4N HCl solution (22 mL) was added to the reaction mixture dropwise and stirred at 0° C. for 20 minutes and then at room temperature overnight. The solution was concentrated in vacuo to give 24 as a yellow solid in 96% yield. 1H NMR (D2O) δ 8.59 (s, 1H), 8.10 (m, 4H), 7.70 (m, 2H), 7.61 (m, 2H), 5.13 (s, 2H), 3.41 (br m, 2H), 3.12 (br m, 4H), 2.79 (br m, 4H), 1.98 (s, 3H), 1.71 (q, 2H), 1.43 (m, 5H); 13C NMR (D2O): δ 174.5, 131.3, 130.8, 129.8, 128.2, 125.7, 122.5, 119.1, 50.0, 49.7, 49.4, 44.9, 44.1, 36.0, 25.5, 21.9, 20.8, 8.7. HRMS (FAB) calcd for C25H33N3O.2HCl (M+H−2HCl)+ 392.2701, Found 392.2702.

1. stirringstirred at 0° C. for 20 minutes
2. customat room temperature
3. customovernight
4. concentrationThe solution was concentrated in vacuo