反应详情

To a mixture of 900 mg of 4-(N-t-butyloxycarbonylmethyloxyethyl-N-methyl-aminocarbonyl)-3-(4-t-butylphenyl)-1-(4-cyanophenyl)-2-methyl- 2H-pyrazol-5-one and 10 ml of ethanol, 4 drops of concentrated sulfuric acid was added, and the resulting reaction solution was refluxed under heating for 2.5 hours. After the ethanol was removed by evaporation under reduced pressure, water was added, and the reaction solution was extracted with chloroform. The extract was washed with saturated aqueous sodium chloride and dried over anhydrous sodium sulfate. The insolubles were filtered off, and the filtrate was concentrated. The resulting residue was recrystallized in chloroform-ether-hexane to give 440 mg of the title compound as colorless crystals.

1. additionwas added
2. customthe resulting reaction solution
3. temperaturewas refluxed
4. temperatureunder heating for 2.5 hours
5. customAfter the ethanol was removed by evaporation under reduced pressure, water
6. additionwas added
7. extractionthe reaction solution was extracted with chloroform
8. washThe extract was washed with saturated aqueous sodium chloride
9. dry with materialdried over anhydrous sodium sulfate
10. filtrationThe insolubles were filtered off
11. concentrationthe filtrate was concentrated
12. customThe resulting residue was recrystallized in chloroform-ether-hexane