反应详情

Into 250 ml of glacial acetic acid, 19.0 g of 3-(4,5-dimethoxy-2-nitrophenyl)-2-methyl-2-propenoic acid ethyl ester were dissolved; and, with 15.0 g of iron powder and 20 ml of ion-exchanged water being added thereto, the mixture was refluxed under heating for 40 minutes. The resulting reaction liquid was filtered out, the filtrate was concentrated under a reduced pressure, and thus obtained residue was dissolved in ethyl acetate. The resulting solution was successively washed with water, a 5% aqueous sodium hydrogencarbonate solution, and a saturated aqueous sodium chloride solution. After this ethyl acetate solution was left on sodium sulfate anhydride for one night so as to be dried, ethyl acetate was evaporated under a reduced pressure, and the resulting residue was recrystallized from a mixed liquid of hexane/ethanol, whereby 12.5 g of the aimed product were obtained (yield: 78%).

1. temperaturethe mixture was refluxed
2. temperatureunder heating for 40 minutes
3. customThe resulting reaction liquid
4. filtrationwas filtered out
5. concentrationthe filtrate was concentrated under a reduced pressure, and thus obtained residue
6. dissolutionwas dissolved in ethyl acetate
7. washThe resulting solution was successively washed with water
8. waitAfter this ethyl acetate solution was left on sodium sulfate anhydride for one night so as
9. customto be dried
10. customethyl acetate was evaporated under a reduced pressure
11. customthe resulting residue was recrystallized from a mixed liquid of hexane/ethanol