Li Shan-bin
2010
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Journal
Henan Chemical Industry
Abstract
7-amino-3-(1-methyl-1-pyrrolidino)methylceph-3-em-4-carboxylate hydrochloride is synthsized from 7-ACA by five steps:protected by silane,replaced by iodine,displacement,romove the protected group,form salt.The characteristics of the title compound is investigated with HNMR.The effect of some factors such as silane,solvent,and the ratio of raw material on the synthesis the title compound are studied.The result shows that the suitable volume ratio of methylene chloride and cyclopentane is 1∶1;the optimum ratio is 7-ACA∶chlorotrimethylsilane∶imidazole∶N-methyl pyrrole is 1∶2.8∶2.4∶1.5;the silane reactiong temperature is 45 ℃,the reaction time is 2.5 h;the reaction temperature of displacement is-10 ℃,the reaction time is 2 h;the overall yield can acheives 96%.