反应详情

To isopropenyl chloride carbonate (6.68 g) were added 4-nitrophenol (5 g) and chloroform (150 ml), and thereto was added drowpise pyridine (2.9 ml) under ice-cooling over a period of 20 minutes. Then, the mixture was stirred under ice-cooling for 15 minutes, then warmed to room temperature, and further stirred overnight. After the reaction was completed, the reaction solution was washed succesively with 1N aqueous hydrochloric acid solution, water and a satureated aqueous sodium chloride solution, dried over magnesium sulfate, filtered and concentrated. The obtained residue was purified by column chromatography (hexane:ethyl acetate=4:1) to give the title compound (1.41 g).

1. temperaturecooling over a period of 20 minutes
2. temperaturecooling for 15 minutes
3. stirringfurther stirred overnight
4. washthe reaction solution was washed succesively with 1N aqueous hydrochloric acid solution, water
5. dry with materiala satureated aqueous sodium chloride solution, dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate=4:1)