Sodium Bicarbonate → HCID 89782865, 화합물

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A vial was charged with a mixture of 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-6-(trifluoromethyl)-1H-indazole (0.05 g, 0.160 mmol), 6-amino-5-bromo-3-methylpyrimidin-4(3H)-one (0.042 g, 0.208 mmol) and PdCl2(dppf) (5.86 mg, 8.01 μmol) in dioxane (8 mL) and aqueous saturated NaHCO3 (2 mL). The resulting light brown suspension was heated at 140° C. for 45 minutes in a microwave reactor. The reaction mixture was subsequently concentrated and the crude residue was purified by preparative HPLC, eluting with a gradient of 25-35% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA) over a period of 4 minutes. The product-containing fractions were combined and the volatiles removed in vacuo to give a TFA salt of the title compound (8 mg, 16%). 1H NMR (400 MHz, CD3OD) δ ppm 3.45 (s, 3H), 7.33 (d, J=1.01 Hz, 1H), 7.83 (s, 1H), 7.89 (d, J=0.76 Hz, 1H), 8.19 (s, 1H); ESI-MS m/z [M+H]+ calc'd for C13H10F3N5O, 310.1. found 310.2.

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