反应详情

To a solution of (E)-[2-(3-{4-[1-(4-bromo-phenylcarbamoyl)-3-(tert-butyl-dimethyl-silanyloxy)-propyl]-phenyl}-acryloylamino)-phenyl]-carbamic acid tert-butyl ester (1.6 g, 2.26 mmol) in THF (40 mL) was added tetrabutylammonium dihydrogen trifluoride (1.36 g, 4.52 mmol). This mixture was stirred at room temperature overnight and then evaporated to remove THF. The mixture was dissolved in water and extracted with ethyl acetate (3×30 mL). The combined organic layer was washed with brine, dried with Na2SO4, filtered, and evaporated. The crude product was purified by column chromatography (CH2Cl2:EtOAc=10:1) to get yellow solid product. MS: calc'd 594 (MH+), exp 594 (MH+).

1. customevaporated
2. customto remove THF
3. dissolutionThe mixture was dissolved in water
4. extractionextracted with ethyl acetate (3×30 mL)
5. washThe combined organic layer was washed with brine
6. dry with materialdried with Na2SO4
7. filtrationfiltered
8. customevaporated
9. customThe crude product was purified by column chromatography (CH2Cl2:EtOAc=10:1)
10. customto get yellow solid product