反应详情

温度

120 °C

(S)-tert-Butyl (3-(benzyloxy)-1-(5-bromo-4-oxo-3-phenyl-3,4-dihydropyrrolo[2,1-f][1,2,4]triazin-2-yl)propyl)carbamate (0.6 g, 1.08 mmol) was dissolved in 36 mL anhydrous dimethylformamide in a pressure reactor vessel. 2,4,6-Trimethylboroxine (1.36 mL, 9.76 mmol), potassium carbonate (3 g, 21.68 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.13 g, 0.11 mmol) were added under argon conditions. The reaction mixture was heated at 120° C. for 2 h and then cooled and filtered through a plug of Celite, washing several times with ethyl acetate. The combinated filtrates were washed with water, saturated ammonium chloride solution and brine, dried over sodium sulphate, filtered and evaporated under reduced pressure. The residue was purified using SP1® Purification System (0% to 20%, hexane-ethyl acetate) to give 0.45 g (85% yield) of the title compound as a white solid.

1. temperaturecooled
2. filtrationfiltered through a plug of Celite
3. washwashing several times with ethyl acetate
4. washThe combinated filtrates were washed with water, saturated ammonium chloride solution and brine
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. customevaporated under reduced pressure
8. customThe residue was purified
9. customSP1® Purification System (0% to 20%, hexane-ethyl acetate)