反应详情

温度

90 °C

A 4 M hydrogen chloride-1,4-dioxane solution (4.5 mL) was added to a suspension of 6-{(E)-2-cyclopentyl-1-[4-(methylsulfanyl)phenyl]ethenyl}-3-cyclopropyl-2-methoxypyridine (150 mg) in water (1.5 mL), and the mixture was stirred at 90° C. for 1.5 hours. The reaction solution was cooled to room temperature and extracted with chloroform twice. 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 dissolved in a hexane-ethyl acetate solution with heating, and then recrystallization by cooling to room temperature gave the title compound as a colorless powder (111 mg, 77%).

1. temperatureThe reaction solution was cooled to room temperature
2. extractionextracted with chloroform twice
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationafter which the filtrate was concentrated under reduced pressure
7. dissolutionThe resulting residue was dissolved in a hexane-ethyl acetate solution
8. temperaturewith heating
9. customrecrystallization
10. temperatureby cooling to room temperature