摘要
以3,5-二氯吡啶为原料,经4步反应制得头孢西酮中间体3,5-二氯-4-吡啶酮乙酸。原料经硝化、还原、重氮化水解、缩合反应制得产物。对各步单元反应进行了条件优化,得到了最优反应条件,4步反应收率为57.6%,HPLC含量为97.5%。反应产物结构经~1HNMR和~(13)CNMR确证,整个合成工艺简单、收率高,具有很好的工业应用前景。
The target compound 3,5-dichloropyridine acetic acid is an important intermediate of Cefasidone which can be prepared from 3,5-dichloropyridine via nitrification,reduction,diazo hydrolysis and condensation.The optimum reaction conditions were obtained,the overall yield of four steps reaction was 57. 6% and the purity of final product was 97. 5%.The structure was confirmed by1 HNMR and13 CNMR.The smooth synthetic process with high yield made it suitable for industrial application.
引文
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