反应详情

温度

90 °C

To a suspension of of 4-(5-bromo-pyridin-3-yl)-2-(6-methyl-pyridin-2-yl)-7H-pyrrolo[2,3-d]pyrimidine (Example 16) (1 eq, 0.451 mmol, 250 mg) in TEA/DMF (1:1, 6 ml) are added copper (I) iodide (0.1 eq, 0.045 mmol, 8.8 mg), PdCl2(PPh3)2 (0.1 eq, 0.045 mmol, 32.3 mg), and trimethylsilylacetylene (Sigma-Aldrich, St. Louis, USA) (1.5 eq, 0.68 mmol, 0.098 ml). The resulting mixture is stirred at 90° C. for 1 h. The solvents are removed in vacuo, then sat. aqueous NaHCO3 solution is added, and the mixture is extracted with EtOAc. The organic layer is washed with sat. aqueous NaCl solution, dried with MgSO4, and concentrated under reduced pressure. The crude product is purified by reversed phase HPLC and recrystallized in EtOAc giving the title compound; [M+H]+=384.

1. customThe solvents are removed in vacuo
2. additionsat. aqueous NaHCO3 solution is added
3. extractionthe mixture is extracted with EtOAc
4. washThe organic layer is washed with sat. aqueous NaCl solution
5. dry with materialdried with MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe crude product is purified by reversed phase HPLC
8. customrecrystallized in EtOAc giving the title compound