反应详情

2,2,2-Trichloroethyl 7-(N-methoxy-2-phenoxyacetamido)-3-methyl-3-cephem-4-carboxylate (490 mg) is dissolved in a mixture of methylene chloride (15 ml), acetic acid (4 ml) and dimethylformamide (4 ml), and under ice-cooling, zinc dust (400 mg) is added. The mixture is stirred at room temperature for 1.5 hours, at the end of which time acetic acid (10 ml), dimethylformamide (2 ml) and zinc dust (300 mg) are further added and stirred for another 1.5 hours. The reaction mixture is diluted with ethyl acetate and filtered. The filtrate is washed with 0.5 N-HCl and aqueous sodium chloride in that order, dried over magnesium sulfate and concentrated. The resultant crude crystals are washed with ether-ethyl acetate to give 7-(N-methoxy-2-phenoxyacetamido)-3-methyl-3-cephem-4-carboxylic acid (141 mg).

1. temperatureunder ice-cooling
2. additionare further added
3. filtrationfiltered
4. washThe filtrate is washed with 0.5 N-HCl and aqueous sodium chloride in that order
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. washThe resultant crude crystals are washed with ether-ethyl acetate