反应详情

温度

-20 °C

To a solution of 371 mg of sodium 7β-[2-(5-amino-1,2,4-thiadiazol-3-yl)-(Z)-2-methoxyiminoacetamido]-3-hydroxymethyl-3-cephem-4-carboxylate and 309 mg of 2-amidinomethylthio-5-mercapto-1,3,4-thiadiazole in 10 ml of DMF was added 600 mg of ethyl o-phenylenephosphate under stirring at -20° C. After stirring at -20° C. to 0° C. for 60 minutes, the mixture was 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 the resultant solid was dissolved in dilute hydrochloric acid. This aqueous solution was subjected to a column chromatography on XAD-II (150 ml), being washed with water and eluted with 30% aqueous ethanol. The eluate was concentrated under reduced pressure and lyophilized to give 381 mg of the title compound as a colorless powder.

1. stirringAfter stirring 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. dissolutionthe resultant solid was dissolved in dilute hydrochloric acid
6. washbeing washed with water
7. washeluted with 30% aqueous ethanol
8. concentrationThe eluate was concentrated under reduced pressure