反应详情

Using ethereal HCl and methanol, the product from Step B (0.73 g, 2.5 mmol) was converted to its hydrochloride salt (136 mg, 17%, 98.4% AUC HPLC) as a white amorphous solid: mp 210-214° C.; 1H NMR (300 MHz, CD3OD) δ 7.76-7.90 (m, 4H), 7.47-7.55 (m, 2H), 7.26 (dd, J=8.6, 1.6 Hz, 1H), 7.10-7.21 (m, 2H), 6.77 (d, J=7.3 Hz, 1H), 4.78 (dd, J=11.2, 6.0 Hz, 1H), 4.65 (d, J=15.7 Hz, 1H), 4.48 (d, J=15.6 Hz, 1H), 3.87 (dd, J=12.1, 6.0 Hz, 1H), 3.66 (t, J=11.8 Hz, 1H), 3.13 (s, 3H), 2.36 (s, 3H), IR (KBr) 3434, 2926, 2546, 1459, 754, 479 cm−1; Cl MS m/z 288 [C21H21N+H]+; Anal. Calcd. for C21H21N.HCl.0.5H2O: C, 75.77; H, 6.96; N, 4.21. Found: C, 76.04; H, 6.85; N, 4.14.