Methanesulfonic Acid → HCID 178505350, compound

Participants

Reaction Steps

To a solution of carboxamide 71 (120 mg, 0.247 mmole) in EtOH (10 mL) was added methanesulfonic acid (48 mg, 0.495 mmole) at room temperature and the reaction mixture was stirred for 15 min. The solvent was removed in vacuo. The residue was dissolved in water (10 mL) and lyophilized to afford methanesulfonic acid salt 72 (160 mg, 95%) as a yellow solid: 1H NMR (300 MHz, DMSO-d6) δ 10.44 (s, 1H), 9.15 (br s, 1H), 8.86 (br s, 1H), 8.72 (br s, 1H), 8.22 (dd, J=8.1, 0.9, Hz, 1H), 8.03 (d, J=8.1 Hz, 1H), 7.80 (br s, 4H), 7.61-7.49 (m, 3H), 7.42 (br s, 2H), 7.28 (d, J=7.8 Hz, 1H), 6.89 (d, J=7.8 Hz, 1H), 4.22 (t, J=5.7 Hz, 2H), 3.35-3.33 (m, 2H), 3.17-2.99 (m, 4H), 2.32 (s, 6H), 2.20-2.10 (m, 2H), 1.68 (br s, 4H); ESI-MS m/z 485 [C23H29ClN8O2+H]+.

Provenance & Evidence