Hydrochloric Acid → HCID 178478752, compound

Participants

Reaction Steps

A solution of compound 6 (0.23 g, 0.539 mmol) in methanol (10 mL) was treated with 1 N HCl solution (10 mL) and the resulting mixture was refluxed for 30 min. The reaction was brought to room temperature and solvent was evaporated. The crude was dissolved into water (10 mL), filtered and washed with water (2×5 mL). The combined water layer was evaporated to obtain compound 54 (0.18 g, 84%) as dihydrochloride salt. 1H NMR (DMSO-d6) δ 11.21 (s, 1H), 9.64 (s, 1H), 9.20-9.04 (m, 2H), 8.60 (s, 1H), 8.15-8.12 (m, 2H), 7.36 (t, 1H, J=4.5 Hz), 7.11-7.03 (m, 2H), 6.66 (d, 1H, J=8.4 Hz), 3.86-3.74 (m, 1H), 3.44-3.32 (m, 4H), 3.06-2.92 (m, 4H), 1.98-1.78 (m, 4H); ESI-MS (m/z, %) 327 (MH+, 100), 244 (81); ESI-HRMS calculated for C18H23N4S (MH+), calculated: 327.1637; observed: 327.1636; HPLC purity: 98.86% by area.

Provenance & Evidence