反应详情

温度

30 °C

A mixture of methyl(triphenyl)phosphonium bromide (111 mg, 0.311 mmol) and potassium tert-butoxide (35 mg, 0.311 mmol) in 1,4-dioxane (2 mL) was stirred at 30° C. for 30 minutes. 2,2,2-trifluoro-N-(3-oxo-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-2) (60 mg, 0.104 mmol) in 1,4-dioxane (2 mL) was added, and the mixture was stirred at room temperature for 15 hours. To the mixture was added NH4Cl, extracted with EtOAc, washed with water and brine, dried (MgSO4), filtered, and the solvent was removed under reduced pressure. The residue was purified by column chromatography eluting with 0-10% methanol in CHCl3 to give 2,2,2-trifluoro-N-(3-methylene-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-11) as a white solid.

1. stirringthe mixture was stirred at room temperature for 15 hours
2. extractionextracted with EtOAc
3. washwashed with water and brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent was removed under reduced pressure
7. customThe residue was purified by column chromatography
8. washeluting with 0-10% methanol in CHCl3