反应详情

TFA (1 mL) was added to a solution of tert-butyl 3-(4-((4-(2-(2-amino-2-oxoethyl)phenethyl)-5-methylpyrimidin-2-yl)amino)phenyl)azetidine-1-carboxylate (A123) (0.087 g, 0.17 mmol) in DCM (3 mL) and the resulting mixture stirred at room temperature for 3 hours. The volatiles were removed in vacuo then 2 M aqueous K2CO3 solution (5 mL) and water (15 mL) were added to the residue. The resulting suspension was sonicated for 1 minute, filtered and the filter cake dried. The resulting residue was purified by semi preparative HPLC to give the title compound 32 as a light tan solid (7.6 mg, 10%); 1H NMR (300 MHz, d4-MeOH) δ 8.12 (s, 1H), 7.74 (d, J=8.6 Hz, 2H), 7.33 (d, J=8.6 Hz, 2H), 7.18-7.28 (m, 4H), 4.31-4.39 (m, 2H), 4.19-4.27 (m, 3H), 3.66 (s, 2H), 3.13-3.18 (m, 2H), 2.96-3.01 (m, 2H), 2.12 (s, 3H). LCMS-B: rt 4.725 min; m/z 402 [M+H]+.

1. customThe volatiles were removed in vacuo
2. addition2 M aqueous K2CO3 solution (5 mL) and water (15 mL) were added to the residue
3. customThe resulting suspension was sonicated for 1 minute
4. filtrationfiltered
5. customthe filter cake dried
6. customThe resulting residue was purified by semi preparative HPLC