反应详情

温度

60 °C

As shown in Scheme 31 to a solution of 1-[4-(1-bromo-1-phenyl-methylene)-piperidin-1-yl]-2-(4,7-dimethoxy-6-azaindol-3-yl)-ethane-1,2-dione (0.094 g, 0.195 mmol), PdCl2(PhCN)2 (0.005 g, 0.0117 mmol), and CuI (0.005 g, 0.0252 mmol) in piperidine (1.5 mL) was added trimethylsilylacetylene (0.070 mL, 0.495 mmol). The mixture was heated at 60° C. for 2 h and the solvent removed in vacuo. The residue was diluted with EtOAc and H2O, the organic phase was separated and the aqueous phase was re-extracted with EtOAc (×2). The combined organic layers were washed, (H2O, brine), dried (Na2SO4) and evaporated, and the residue was purified by preparative HPLC to give the title compound as a colorless solid (0.038 g, 39%).

1. customthe solvent removed in vacuo
2. additionThe residue was diluted with EtOAc and H2O
3. customthe organic phase was separated
4. extractionthe aqueous phase was re-extracted with EtOAc (×2)
5. washThe combined organic layers were washed, (H2O, brine),
6. dry with materialdried (Na2SO4)
7. customevaporated
8. customthe residue was purified by preparative HPLC