Hydrochloric Acid → HCID 118235654, compound

Participants

Reaction Steps

A solution of Example 320 (92%, 346 mg, 0.573 mmol) in 1,4-dioxane (3 mL) was treated with 4M hydrogen chloride in 1,4-dioxane (2.8 mL). The mixture was placed in a sonic bath for 15 minutes, then stirred at room temperature for 2 h to give a suspension. The reaction mixture was concentrated under vacuum, and purified by preparative HPLC (Method A), to afford the title compound (36 mg, 12.5%) as a colourless solid. δH (500 MHz, CD3OD) 9.05 (d, J 1.4 Hz, 2H), 8.38 (d, J 7.1 Hz, 1H), 8.23 (s, 1H), 7.41 (d, J 10.8 Hz, 1H), 7.33-7.27 (m, 1H), 7.18 (d, J 8.0 Hz, 1H), 7.16-7.12 (m, 1H), 7.11 (dd, J 7.7, 1.8 Hz, 1H), 6.91 (t, J 74.0 Hz, 1H), 4.64 (d, J 11.8 Hz, 2H), 4.42 (s, 2H), 4.33 (d, J 11.8 Hz, 2H), 2.42 (s, 3H). Method D HPLC-MS: MH+ m/z 456, RT 0.98 minutes.

Provenance & Evidence