反应详情

温度

150 °C

A suspension of 2-(2-(2-(2-chloro-5-methylpyrimidin-4-yl)ethyl)phenyl)acetamide (K6) (200 mg, 0.690 mmol), Pd(OAc)2(16 mg, 0.069 mmol), Xantphos (59.9 mg, 0.104 mmol), Cs2CO3 (648 mg, 1.99 mmol) and N-(3-(4-aminophenyl)oxetan-3-yl)-2-methylpropane-2-sulfinamide (A121) (204 mg, 0.759 mmol) in 1,4-dioxane (1.73 mL) was heated under microwave irradiation for 10 minutes at 150° C. under nitrogen. The resulting mixture was filtered through Celite, washing with EtOAc. The volatiles were removed in vacuo and the residue was purified by silica gel column chromatography (CombiFlash Rf, SiO2 cartridge, 0-30% MeOH in DCM) to give the title compound A122 (102 mg, 28%); 1H NMR (300 MHz, d4-MeOH) δ 8.07 (s, 1H), 7.74 (d, J=8.6 Hz, 2H), 7.35 (d, J=8.7 Hz, 2H), 7.19 (m, 4H), 5.17 (d, J=6.6 Hz, 1H), 5.07 (d, J=6.5 Hz, 1H), 5.03 (d, J=6.7 Hz, 1H), 4.93 (d, J=6.4 Hz, 1H), 3.64 (s, 2H), 3.12 (m, 2H), 2.95 (m, 2H), 2.07 (s, 3H), 1.27 (s, 9H). LCMS-B: rt 5.80 min; 522.2 m/z [M+H]+.

1. filtrationThe resulting mixture was filtered through Celite
2. washwashing with EtOAc
3. customThe volatiles were removed in vacuo
4. customthe residue was purified by silica gel column chromatography (CombiFlash Rf, SiO2 cartridge, 0-30% MeOH in DCM)