Synthesis of a Crystal Compound of Cephalosporin Nucleate Hydroiodate
Prepare trimethyliodosilane by reacting hexamethyldisilane with iodine in a solvent.After silanization protection of 7-aminocephalosporin acid(7-ACA)and hexamethyldisilazane(HMDS)catalyzed by imidazolium hydroiodide,trimethylchlorosilane and N,N-diethylaniline were added.Add trimethyliodosilane for the halogenation reaction,then add pyridine for substitution reaction,add solvent and use water quenching to obtain a mixture of 7-amino-3-(1-pyridylmethyl)cephalosporin acid iodide and hydrogen chloride;The mixture is dissolved and faded by adding acid,potassium iodide is then added,and the pH is adjusted by alkaline solution for crystallization;This process obtains a crystal like compound of white 7-amino-3-(1-pyridylmethyl)cephalosporin hydroiodate.The compound purity is of 99.28％(HPLC),PXRD detection has crystalline characteristics and good acceleration stability.
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