反应详情

温度

140 °C

4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-6-(trifluoromethyl)-1H-indazole (39.5 mg, 0.127 mmol), 5-bromopyridine-2-sulfonamide (45 mg, 0.190 mmol), PdCl2(dppf) (9.26 mg, 0.013 mmol), sodium bicarbonate (0.271 mL, 0.506 mmol), and dioxane (2 mL) were mixed in a 10 mL vial to give an orange suspension. The vial was sealed and then heated to 140° C. for 20 minutes in a microwave reactor. The reaction mixture was subsequently filtered and the product was purified by preparative HPLC, eluting with a gradient of 35-60% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA). The pure fractions were lyophilized to give a TFA salt of the title compound as a white solid (9.9 mg, 17%). 1H NMR (400 MHz, CD3OD) δ ppm 2.01 (s, 1H), 7.61 (d, J=1.26 Hz, 1H), 8.03 (s, 1H), 8.17-8.21 (m, 1H), 8.34 (d, J=1.01 Hz, 1H), 8.43 (dd, J=8.08, 2.27 Hz, 1H), 9.07 (dd, J=2.27, 0.76 Hz, 1H); ESI-MS m/z [M+H]+ calc'd for C13H9F3N4O2S, 343.0. found 343.2.

1. customto give an orange suspension
2. customThe vial was sealed
3. filtrationThe reaction mixture was subsequently filtered
4. customthe product was purified by preparative HPLC
5. washeluting with a gradient of 35-60% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA)