反应详情

Pd(PPh3)4 (4 mg, 0.0037 mmol) was added to a mixture (S)-2-(5-bromo-2,7-dimethylquinolin-6-yl)-2-tert-butoxyethyl pivalate (5E) (16 mg, 0.037 mmol), 2,3-dihydropyrano[4,3,2-de]quinolin-7-ylboronic acid hydrochloride (6A) (23 mg, 0.073 mmol) and K2CO3 (0.083 mL 2 M in water, 1.66 mmol) in 1,2-dimethoxyethane (2 mL). The reaction mixture was flushed with nitrogen, microwaved at 120° C. for 90 min and the volatile component was removed in vacuo. The residue was dissolved in ethyl acetate (50 mL), washed with NaHCO3 solution, water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was purified by prep-HPLC to provide 6B as a white solid (4 mg as TFA salt, 18%). LCMS-ESI+ (m/z): 527.3 (M+H)+.

1. customThe reaction mixture was flushed with nitrogen
2. custommicrowaved at 120° C. for 90 min
3. customthe volatile component was removed in vacuo
4. dissolutionThe residue was dissolved in ethyl acetate (50 mL)
5. washwashed with NaHCO3 solution, water and brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe obtained residue was purified by prep-HPLC