反应详情

温度

85 °C

48% hydrobromic acid (1.5 mL) was added to a solution of 3-chloro-6-{(E)-2-cyclopentyl-1-[4-(methylsulfanyl)phenyl]ethenyl}-2-methoxypyridine (250 mg) in 1,4-dioxane (1.5 mL), and the mixture was stirred at 85° C. for one hour. The reaction solution was poured into water, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered, after which the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=9:1) to give a pale brown oil. This was powdered with a hexane/ethyl acetate solution, and filtration operation gave the title compound as a pale brown powder (230 mg, 71%).

1. extractionfollowed by extraction with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationafter which the filtrate was concentrated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (chloroform:methanol=9:1)
7. customto give a pale brown oil
8. filtrationThis was powdered with a hexane/ethyl acetate solution, and filtration operation