反应详情

To a mixture of (5-bromo-2-ethylthiophen-3-yl)(cyclohexyl)methanol (1.50 g) synthesized above, methyl 4-hydroxybenzoate (904 mg), 1,1′-(azodicarbonyl)dipiperidine (2.50 g) and tetrahydrofuran (30 mL) was added tributylphosphine (2.47 mL), and the mixture was stirred at room temperature for 3 hr. The reaction mixture was concentrated under reduced pressure, and the precipitate was removed by filtration and washed with diisopropyl ether. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9, volume ratio) to give the title compound (1.20 g, 55%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customthe precipitate was removed by filtration
3. washwashed with diisopropyl ether
4. concentrationThe filtrate was concentrated under reduced pressure
5. customthe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9, volume ratio)