反应详情

温度

80 °C

To a mixture of 4-methoxy-7-bromo-6-azaindole (0.200 g, 0.88 mmol), PdCl2(PhCN)2 (0.017 g, 0.044 mmol), tri-2-furylphosphine (0.0410 g, 0.176 mmol) and CuI (0.017 g, 0.088 mmol) was added piperidine (10 mL), followed by 3-butyn-2-ol (0.09 mL, 1.15 mmol). The mixture was heated at 80° C. for 6 h and then the solvent was removed in vacuo. The residue was partitioned with EtOAc-H2O and then the aqueous phase was separated and re-extracted with EtOAc (×2). The combined organic layers were washed (H2O, brine), dried (Na2SO4) and concentrated to afford the title compound (0.200 g, 95%) as a brown solid which was of sufficient purity for use in the following step:

1. customthe solvent was removed in vacuo
2. customThe residue was partitioned with EtOAc-H2O
3. customthe aqueous phase was separated
4. extractionre-extracted with EtOAc (×2)
5. washThe combined organic layers were washed (H2O, brine)
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated