反应详情

温度

-20 °C

To a solution of 363 mg of sodium 7β-[2-(2-aminothiazol-4-yl)-(Z)-2-methoxyiminoacetamido]-3-hydroxymethyl-3-cephem-4-carboxylate and 241 mg of 1-(3-guanidinopropyl)-5-mercapto-1H-tetrazole in 10 ml of DMF was added 800 mg of ethyl o-phenylenephosphate under stirring at -20° C. The reaction mixture was stirred at -20° C. to 0° C. for 60 minutes and subjected to a column chromatography on silica gel (100 g), being washed with acetonitrile and eluted with acetonitrile/water (4:1). The eluate was concentrated under reduced pressure and subjected to a column chromatography on XAD-II (150 ml), being washed with water and eluted with 20% aqueous ethanol. The eluate was concentrated under reduced pressure and then lyophilized to give 294 mg of the title compound as a colorless powder.

1. stirringThe reaction mixture was stirred at -20° C. to 0° C. for 60 minutes
2. washbeing washed with acetonitrile
3. washeluted with acetonitrile/water (4:1)
4. concentrationThe eluate was concentrated under reduced pressure
5. washbeing washed with water
6. washeluted with 20% aqueous ethanol
7. concentrationThe eluate was concentrated under reduced pressure