反应详情

This compound was prepared via the general DCC/pyr coupling procedure from 8 (1.4886 g, 5.97 mmol), 2-nitrophenylacetic acid (2.1619 g, 11.93 mmol), DCC(2.5402 g, 12.31 mmol), and pyridine (1.00 mL, 12.36 mmol). The crude product was converted to the HCl salt with Et2O—HCl without chromatography and crystallized from MeOH—Et2O. The first crop was recrystallized again from MeOH—Et2O to yield 10 HCl.(1.3663 g, 51%): m.p. (HCl salt) 258-259° C.; 1H NMR (HCl salt, DMSO-d6) δ1.97 (br s, 4H, —CH2CH2—), 2.91 (s, 3H, —NCH3), 3.11-4.45 (complex, 8H, 4 —CH2—), 6.17 (m, 1H, —CH—), 7.51-8.25 (complex, 8H, aromatic). MS(FAB) m/z 413. Anal. (C, H, N) C21H24N4O5.HCl.0.25H2O.

1. customcrystallized from MeOH—Et2O
2. customThe first crop was recrystallized again from MeOH—Et2O