反应详情

温度

75 °C

A mixture of 6-(1-(6-bromo-[1,2,4]triazolo[4,3-a]pyridin-3-yl)ethyl)-N-(2,4-dimethoxybenzyl)pyridazin-3-amine (750 mg, 1.598 mmol), anisole (0.349 mL, 3.20 mmol), and TFA (1.0 mL, 12.98 mmol) in DCM (5.0 mL) was heated in a microwave on high absorbance for 2 hrs at 75° C. The reaction was stripped to dryness via rotary evaporation, and the resulting oil was treated with Et2O to produce a solid. The solid was filtered and dried under vacuum to provide the title compound, 6-(1-(6-bromo-[1,2,4]triazolo[4,3-a]pyridin-3-yl)ethyl)pyridazin-3-amine 2,2,2-trifluoroacetate (400 mg, 0.923 mmol, 57.8% yield) as a yellow solid. 1H NMR 48F (400 MHz, DMSO-d6) δ ppm 1.77 (d, J=7.07 Hz, 3 H) 5.05 (d, J=7.07 Hz, 1 H) 7.44 (d, J=9.60 Hz, 1 H) 7.50 (dd, J=9.73, 1.64 Hz, 1 H) 7.73-7.84 (m, 1 H) 7.92 (d, J=9.60 Hz, 1 H) 8.56 (br. s., 2 H) 8.81 (s, 1 H). ESI-MS:m/z 319.1 (M+H)+.

1. customThe reaction was stripped to dryness via rotary evaporation
2. additionthe resulting oil was treated with Et2O
3. customto produce a solid
4. filtrationThe solid was filtered
5. customdried under vacuum