反应详情

A mixture of tert-Butyl 4-(3-(8-(5,6-dimethoxypyridin-2-ylamino)imidazo[1,2-b]pyridazin-6-yl)benzamido)benzoate (80 mg, 0.14 mmol) and TFA (3 mL) in dichloromethane (3 mL) was stirred for 2 h at room temperature. The mixture was concentrated and then triturated with MeOH (2 mL) to give the product 4-(3-(8-(5,6-dimethoxypyridin-2-ylamino)imidazo[1,2-b]pyridazin-6-yl)benzamido)benzoic acid (28 mg, 39%) as a yellow solid. 1H NMR (300 MHz, DMSO): δ 10.71 (s, 1H), 10.02 (s, 1H), 8.66 (s, 1H), 8.55 (s, 1H), 8.29 (s, 1H), 8.24 (d, 1H, J=7.8 Hz), 8.12 (d, 1H, J=7.5 Hz), 7.97-7.93 (m, 2H), 7.76-7.71 (m, 3H), 7.44 (d, 1H, J=8.1 Hz), 7.13 (d, 1H, J=8.4 Hz), 4.05 (s, 3H), 3.88 (s, 3H). LC-MS: [M+H]+, 510.9, tR=1.505 min, HPLC: 97.21% at 214 nm, 99.12% at 254 nm, tR=6.006 min.

1. concentrationThe mixture was concentrated
2. customtriturated with MeOH (2 mL)