反应详情

To a solution of tert-butyl 3-(2-fluoro-4-{[(4′-hydroxy-2′,6′-dimethylbiphenyl-3-yl)methyl][(2-nitrophenyl)sulfonyl]amino}phenyl)propanoate (1.2 g, 1.89 mmol), 1-(2-hydroxyethyl)pyrrolidin-2-one (0.23 mL, 2.08 mmol) and tributylphosphine (0.75 mL, 2.84 mmol) in tetrahydrofuran (25 mL) was added 1,1′-(azodicarbonyl)dipiperidine (0.74 g, 2.84 mmol) under stirring at room temperature, and the mixture was stirred for 14 hr. The resulting precipitate was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1-ethyl acetate) to give the title compound (0.91 g, yield 65%) as a colorless oil.

1. stirringthe mixture was stirred for 14 hr
2. filtrationThe resulting precipitate was filtered off
3. concentrationthe filtrate was concentrated under reduced pressure
4. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1-ethyl acetate)