Trifluoroacetic acid → HCID 12210169, compound

Participants

Reaction Steps

A solution of 2-amino-3-methoxybenzoic acid (10.1 g, 60.4 mmol) in acetic anhydride (50 ml, 530 mmol) was heated to 140° C. with stirring for 180 min. The reaction mixture was cooled to room temperature and concentrated to provide Intermediate A-9A (11.51 g, 100%): 1H NMR (400 MHz, DMSO-d6) δ 7.59 (dd, J=6.9, 2.3 Hz, 1H), 7.52-7.42 (m, 2H), 3.89 (s, 3H), 2.39 (s, 3H); HPLC: RT=0.795 min (H2O/MeOH with TFA, SunFire C18 2.5 μm, 2.1×30 mm, gradient=2 min, wavelength=220); MS(ES): m/z=292 [M+H]+.

Provenance & Evidence