Hydrochloric Acid → HCID 25140023, compound

Participants

Reaction Steps

A mixture of acetate 122 (5.60 g, 19.2 mmol) and 5 M HCl (80 mL) in MeOH (80 mL) was stirred at reflux temperature for 30 min. The solvent was evaporated to give the hydrochloride salt of 123 (4.42 g, 94%) as an orange solid: mp (MeOH) 143-145° C.; 1H NMR [(CD3)2SO] δ 7.73 (s, 1H, H-7), 7.43 (br s, 4H, NH2, OH, HCl), 6.84 (s, 1H, H-4), 3.31-3.38 (m, 2H, CH2O), 2.77-2.90 (m, 2H, CH2), 2.44-2.64 (m, 3H, CH2, CH); 13C NMR [(CD3)2SO] δ 153.2, 145.7 131.4, 129.1, 119.8, 113.7, 63.8, 41.5, 35.2, 33.6; HRMS calcd for C10H12N2O3 (M+) m/z 208.0848, found 208.0850. Anal. calcd for C10H12N2O3.HCl: C, 49.1; H, 5.4; N, 11.5. Found: C, 49.4; H, 5.4; N, 11.5%.

Provenance & Evidence