反应详情

Into a reaction flask were added tert-butyl (5-bromopyridin-3-yl)carbamate (3.0 g, 11.0 mmol), tetrahydrofuran (30 mL), and triethylamine (1.7 mL, 12 mmol). The reaction mixture was stirred under N2 bubbling for 5 min. (Trimethylsilyl)acetylene (1.60 g, 16.3 mmol), copper(I) iodide (84 mg, 0.44 mmol), and bis(triphenylphosphine)palladium(II) chloride (0.31 g, 0.44 mmol) were then added. The resultant mixture was heated at 50° C. overnight. The solvent was removed under vacuum and the residue was diluted with EtOAc and water. After separation, the organic layer was dried over Na2SO4 and concentrated under vacuum. The crude product was purified by silica gel column chromatography to give the desired product as a white powder (2.0 g, 63%). LCMS for C15H23N2O2Si (M+H)+: m/z=291.1.

1. additionwere then added
2. customThe solvent was removed under vacuum
3. additionthe residue was diluted with EtOAc and water
4. customAfter separation
5. dry with materialthe organic layer was dried over Na2SO4
6. concentrationconcentrated under vacuum
7. customThe crude product was purified by silica gel column chromatography