反应详情

7β-Amino-3-[2-(N-carboethoxysulfamoyl)benzoyloxy]methyl-3-cephem-4-carboxylic acid (457 mg) is suspended in a mixed solution of dichloromethane (5 ml) and N,N-dimethylformamide (1.0 ml) and to the mixture, a solution of (1H-tetrazol-1-yl)acetyl chloride (161 mg) in tetrahydrofuran (2 ml) is added over a period of 20 minutes and stirred for 2 hours. The solvent is distilled off under reduced pressure and to the resultant viscous residue, ethyl acetate (50 ml) and water (20 ml) are added and stirred. After separation, the ethyl acetate layer is washed with water, dried over anhydrous sodium sulfate and concentrated. To the concentrate (5 ml), chloroform (50 ml) is added and the resultant precipitate is filtered off. The filtrate is concentrated and to the concentrate (5 ml), ether (50 ml) is added. The resultant precipitate is collected by filtration and dried over phosphorous pentoxide. The procedure provides 7β-(1H-tetrazol-1-yl)acetamido-3-[2-(N-carboethoxysulfamoyl)benzoyloxy]methyl-3-cephem-4-carboxylic acid (216 mg).

1. distillationThe solvent is distilled off under reduced pressure
2. additionto the resultant viscous residue, ethyl acetate (50 ml) and water (20 ml) are added
3. stirringstirred
4. customAfter separation
5. washthe ethyl acetate layer is washed with water
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated
8. concentrationTo the concentrate (5 ml), chloroform (50 ml)
9. additionis added
10. filtrationthe resultant precipitate is filtered off
11. concentrationThe filtrate is concentrated
12. concentrationto the concentrate (5 ml), ether (50 ml)
13. additionis added
14. filtrationThe resultant precipitate is collected by filtration
15. dry with materialdried over phosphorous pentoxide