反应详情

To a solution of ethyl 3-(2-fluoro-4-{[(4′-hydroxy-2′,6′-dimethylbiphenyl-3-yl)methyl]amino}phenyl)propanoate (0.50 g, 1.2 mmol), (3-methoxy-1-methyl-1H-pyrazol-5-yl)methanol (0.17 g, 1.2 mmol) and tributylphosphine (0.59 mL, 2.4 mmol) in tetrahydrofuran (30 mL) was added 1,1′-(azodicarbonyl)dipiperidine (0.60 g, 2.4 mmol), and the mixture was stirred at room temperature for 2 hr. The reaction solution was concentrated, diisopropyl ether was added to the residue, and the resultant insoluble material was filtered off. The filtrate was concentrated and the residue was purified by silica gel column chromatography (40% ethyl acetate/hexane) to give the title compound (0.44 g, yield 68%) as a colorless oil.

1. concentrationThe reaction solution was concentrated
2. additiondiisopropyl ether was added to the residue
3. filtrationthe resultant insoluble material was filtered off
4. concentrationThe filtrate was concentrated
5. customthe residue was purified by silica gel column chromatography (40% ethyl acetate/hexane)