反应详情

TFA (0.5 mL) was added to a solution of 2-(2-(2-(2-(4-(3-(1,1-dimethylethylsulfinamido)oxetan-3-yl)phenylamino)-5-methylpyrimidin-4-yl)ethyl)phenyl)acetamide (A122) (30 mg, 0.058 mmol) in DCM (3.0 mL) under a nitrogen atmosphere and the resulting mixture stirred at room temperature for 30 minutes, then at 35° C. overnight. The volatiles were evaporated under reduced pressure, keeping the temperature below 30° C. The resulting oil was purified by semi preparative HPLC, to give the title compound 31 (5.0 mg, 21%); 1H NMR (300 MHz, d4-MeOH) δ 8.24 (br s, 1H), 8.15 (s, 1H), 7.85 (d, J=8.8 Hz, 2H), 7.38 (d, J=8.8 Hz, 2H), 7.22 (m, 4H), 5.13 (d, J=7.7 Hz, 2H), 4.97 (d, J=7.7 Hz, 2H), 3.67 (s, 2H), 3.16 (m, 2H), 3.00 (m, 2H), 2.13 (s, 3H). LCMS: rt 4.72 min; m/z 418.2 [M+H]+.

1. customat 35° C.
2. customovernight
3. customThe volatiles were evaporated under reduced pressure
4. customthe temperature below 30° C
5. customThe resulting oil was purified by semi preparative HPLC