반응 #194
ord-a6ed7cd19836494cb3c62d6a1e160912
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27/05 2009 13:35:19 +0200 To dry degassed dioxane (30 mL) were added ethyl 7-bromobenzofuran-2-carboxylate (2.30 g, 8.55 mmol) and 1-(2-(pyridin-2-yl)ethyl)piperazine (1.798 g, 9.40 mmol), Cesium carbonate (3.62 g, 11.11 mmol), 2-Dicyclohexylphosphino-2',4',6'-triisopropylbiphenyl (0.407 g, 0.85 mmol) and Tris(dibenzylideneacetone)dipalladium(0) (0.391 g, 0.43 mmol) under argon and the reaction heated at 95°C for 4h. The reaction mixture was filtered and solvent evaporated. The material was purified by flash (SiO2; DCM/MeOH 97/3) to give 0.620 g, but it was not pure enough (EN02198-94-001). A second flash was performed (SiO2; DCM/MeOH 97/3) to give 0.540 g of the product as a yellow solid (EN02198-94-002). 100% pure according to HPLC. The reaction mixture was combined with the reaction mixture in EN02745-56 and hydrolysed.