反应详情

温度

2.5 °C

Amide compound 5 (1.8 g) was dissolved in CH2Cl2 (30 mL) and cooled to 0-5° C. Hydrogen chloride gas was bubbled through this solution for 20 min. The bubbling was discontinued and the reaction mixture was stirred at room temperature for 2 h. The excess HCl was degassed and the CH2Cl2 was removed. The residual sticky solid was dried under vacuum without further purification to yield the crude hydrochloride salt 23 (1.5 g, quantitative yield). 1H NMR (400 MHz, DMSO-d6): 7.20 (overlapped d, J=8.4 Hz, 2H), 7.18 (overlapped d, J=8.4 Hz, 2H), 6.90 (d, J=8.8 Hz, 2H), 6.86 (d, J=8.8 Hz, 2H), 4.50 (m, 1H), 3.55 (s, 3H), 2.98-3.04 (m, 3H), 2.91 (dd, J=14.0 and 8.0 Hz, 1H), 2.80 (t, J=7.2 Hz, 2H), 2.77 (s, 3H), 2.67 (s, 3H), 2.59 (t, J=7.2 Hz, 2H).

1. customHydrogen chloride gas was bubbled through this solution for 20 min
2. customThe excess HCl was degassed
3. customthe CH2Cl2 was removed
4. customThe residual sticky solid was dried under vacuum without further purification