反应详情

温度

80 °C

A mixture of 6-bromo-1-(pentan-3-yl)-1H-imidazo[4,5-b]pyrazin-2-ol (3.75 g, 13.2 mmol)), trimethylsilylacetylene (2.8 mL, 19.8 mmol), PdCl2(PPh)2 (0.93 g, 1.32 mmol), CuI (0.5 g, 2.64 mmol) and triethylamine (5.5 mL, 39.5 mmol) in DMF (50 mL) was purged with N2 for 30 seconds followed by stirring at 80° C. After 3 hours the reaction mixture was diluted with EtOAc, washed with NH4Cl solution, dried over Na2SO4, and concentrated in vacuo. Purification with over silica gel (Biotage MPLC 10-80% EtOAc/hexanes) provided the title compound (3.2 g, 80%) as a brown solid.

1. customwas purged with N2 for 30 seconds
2. additionAfter 3 hours the reaction mixture was diluted with EtOAc
3. washwashed with NH4Cl solution
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customPurification with over silica gel (Biotage MPLC 10-80% EtOAc/hexanes)