HCID 11233520, compound → HCID 86035666, compound

Participants

Reaction Steps

[3-(5-Chloro-2-oxo-2H-1-benzopyran-4-yloxy)-propyl]-carbamic acid tert-butyl ester (24a) (0.079 g, 0.22 mmol) is treated with 4N HCl/dioxane for several minutes during which time a precipitate is formed. The solventVHCl is removed under reduced pressure. The residue is recrystallized from MeOH/EtOAc followed by a second recrystallization from EtOH to afford the title compound as the hydrochloric acid salt (22.8 mg, 41%). 1H NMR (DMSO-d6, 300 MHz) δ 7.94 (3H, brs), 7.62 (1H, t, J=8.25 Hz), 7.43 (2H, m), 5.94 (1H, s), 4.29 (2H, t, J=5.75 Hz), 3.04 (2H, t, J=7 Hz), 2.14 (2H, m); MS (ESI, Pos.) calcd for C12H12ClNO3 m/z [M+H]=254.0, found 254.1.

Provenance & Evidence