反应详情

Sodium 7-[(Z)-2-methoxyimino-2-(thiazol-4-yl)-acetamido]-3-carbamoyloxymethyl-3-cephem-4-carboxylate (100 mg) was dissolved in dimethylformamide (1 ml). 3-Bromophthalide (69 mg) was added to the solution. After stirring for one hour at room temperature, the reaction mixture was added to a mixture of dil. HCl (10 ml) and ethyl acetate (20 ml). The resulting ethyl acetate layer was separated, washed successively with dil. HCl (10 ml) and saturated aqueous NaCl (10 ml×2), dried over anhydrous magnesium sulfate, and concentrated to dryness under reduced pressure. The residue was dissolved in ethyl acetate (2 ml) and the solution was added dropwise to a petroleum ether-diethyl ether mixture (100 ml) with stirring. Resulting crystals well filtered, and dried under reduced pressure to give the title compound (45 mg).

1. customThe resulting ethyl acetate layer was separated
2. washwashed successively with dil. HCl (10 ml) and saturated aqueous NaCl (10 ml×2)
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated to dryness under reduced pressure
5. dissolutionThe residue was dissolved in ethyl acetate (2 ml)
6. additionthe solution was added dropwise to a petroleum ether-diethyl ether mixture (100 ml)
7. stirringwith stirring
8. customResulting crystals
9. filtrationwell filtered
10. customdried under reduced pressure