反应详情

温度

80 °C

9-Bromo-6-(4-methoxybenzyl)pyrido[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5(6H)-one (Example 1, 30 mg, 0.078 mol), potassium (2-(benzyloxycarbonylamino)ethyl)trifluoroborate (30 mg, 0.11 mol), Cs2CO3 (122 mg, 0.38 mmol), PdCl2(dppf)-DCM (5 mg, 0.01 mol), toluene (0.75 mL) and degassed water (0.25 mL) were added in order. The mixture was heated at 80° C. for 16 h, concentrated under a stream of nitrogen. The crude residue was taken up in DMF (1.5 mL), filtered and purified (HPLC, 0-85% ACN in water) to afford the title compound (6 mg, 12%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 2.92 (t, J=5.4 Hz, 2H), 3.35-3.36 (m, 2H), 3.69 (s, 3H), 4.94 (s, 2H), 5.58 (s, 2H), 6.83-6.85 (m, 2H), 7.24-7.26 (m, 2H), 7.35-7.37 (m, 2H), 7.40 (dd, J=4.4, 4.4 Hz, 1H), 8.51 (d, J=1.5 Hz, 1H), 8.61 (s, 1H), 8.65 (d, J=1.6 Hz, 1H). [M+H]=485.2.

1. additionwere added in order
2. concentrationconcentrated under a stream of nitrogen
3. filtrationfiltered
4. custompurified (HPLC, 0-85% ACN in water)