反应详情

To a suspension of methyl 3-[6-amino-5-(1,3-benzothiazol-2-yl)pyridin-3-yl]phenoxyacetate (75 mg, 0.19 mmol) in EtOH (4.0 mL) and H2O (4.0 mL) was added 3M aqueous NaOH (0.30 mL, 1.0 mmol). The reaction mixture was left to stir at rt overnight. Then, the mixture was acidified with 1M HCl aqueous to pH=2. Vacuum filtration afforded the title compound as a yellow solid. 1H NMR (400 MHz, DMSO-d6): δ=4.80 (s, 2H), 6.93 (dd, J=7.7, 2.1 Hz, 1H), 7.25-7.29 (m, 1H), 7.31 (d, J=7.8 Hz, 1H), 7.40 (t, J=7.8 Hz, 1H), 7.48-7.54 (m, 1H), 7.55-7.62 (m, 1H), 8.15 (dd, J=18.4, 7.6 Hz, 2H), 8.31 (d, J=2.0 Hz, 1H), 8.55 (d, J=2.3 Hz, 1H), 13.06 (br. s., 1H). MS (ES+): m/z=378.07 (100) [MH+]. HPLC: tR=3.50 min (ZQ3, polar—5 min).

1. waitThe reaction mixture was left
2. filtrationVacuum filtration