反应详情

TFA (0.5 mL) was added to a cooled (water/ice bath 6° C.) solution of tert-butyl 4-(4-((4-(2-(2-amino-2-oxoethyl)phenethyl)-5-methylpyrimidin-2-yl)amino)phenoxy)piperidine-1-carboxylate (A113) (0.050 g, 0.092 mmol) in DCM (2 mL) and the resulting mixture was stirred at room temperature for 4 hours. The volatiles were removed in vacuo then 2 M aqueous K2CO3 solution (10 mL) and water (10 mL) were added to the residue. The resulting suspension was sonicated for 1 minute, filtered and the filter cake dried to give the title compound 26 as a light pink solid (0.034 g, 83%); 1H NMR (300 MHz, d6-DMSO) δ 9.17 (s, 1H), 8.12 (s, 1H), 7.62 (d, J=8.9 Hz, 2H), 7.43 (s, 1H), 7.12-7.27 (m, 4H), 6.93 (s, 1H), 6.84 (d, J=8.9 Hz, 2H), 4.23-4.29 (m, 1H), 3.49 (s, 2H), 3.30-3.34 (m, 2H), 2.83-3.05 (m, 7H), 2.05 (s, 3H), 1.86-1.90 (m, 2H), 1.39-1.42 (m, 2H). LCMS-B: rt 4.717 min; m/z 446 [M+H]+.

1. customThe volatiles were removed in vacuo
2. addition2 M aqueous K2CO3 solution (10 mL) and water (10 mL) were added to the residue
3. customThe resulting suspension was sonicated for 1 minute
4. filtrationfiltered
5. customthe filter cake dried