Hydrochloric Acid → Hydrochloric Acid

Participants

Reaction Steps

A mixture of Example 309E (4.0 g, 10.14 mmol) and 4M HCl in dioxane (25.4 ml, 101 mmol) in methanol (10 mL) was stirred at room temperature for 4 hours. The mixture was concentrated and the solid was washed with ethyl acetate and vacuum dried to provide the title compound as an HCl salt. 1H NMR (400 MHz, DMSO-d6) δ 2.81 (s, 2H), 3.33 (s, 2H), 3.83 (s, 2H), 6.62 (s, 1H), 7.17 (d, J=1.6 Hz, 1H), 7.30 (dd, J=7.9, 2.6 Hz, 1H), 7.68 (d, J=5.2 Hz, 1H), 8.08-8.25 (m, 2H), 8.37 (d, J=5.2 Hz, 1H), 9.46 (s, 2H), 12.44 (s, 1H). MS (ESI+) m/z 295.1 (M+H)+.

Provenance & Evidence