反应详情

温度

120 °C

To a pressure tube flushed with N2 were added (S)-ethyl 2-(7-(4-(allyloxy)-4-methylpiperidin-1-yl)-2-(((2-bromo-4-(trifluoromethyl)benzyl)oxy)methyl)-5-methylpyrazolo[1,5-a]pyrimidin-6-yl)-2-(tert-butoxy)acetate (0.200 g, 0.281 mmol), acetonitrile (8 ml) and triethylamine (0.392 ml, 2.81 mmol). Added to this solution were triphenylphosphine (0.022 g, 0.084 mmol) and tris(dibenzylideneacetone)dipalladium (0) (0.026 g, 0.028 mmol). The tube was sealed and stirred at 120° C. for 23 h. The mixture was cooled, filtered and concentrated to give a yellow residue that was purified by flash chromatography (Biotage; 0%-100% EtOAc/hexane; 20 CV) to give the title compound (0.1115 g, 0.177 mmol, 62.9% yield) as a yellow foam. LCMS (M+H) calcd for C34H44F3N4O4: 631.31. found: 631.3.

1. customTo a pressure tube flushed with N2
2. additionAdded to this solution
3. customThe tube was sealed
4. temperatureThe mixture was cooled
5. filtrationfiltered
6. concentrationconcentrated
7. customto give a yellow residue that
8. customwas purified by flash chromatography (Biotage; 0%-100% EtOAc/hexane; 20 CV)