红霉素肟的合成新工艺

A New Synthetic Route for Synthesis of Erythromycin Oxime

以硫氰酸红霉素为原料、盐酸羟胺为肟化试剂、氢化钠为碱、甲醇为溶剂合成了红霉素肟盐,经20%氢氧化钠中和、二氯甲烷萃取,最后在30%甲醇溶液中结晶,"一锅法"得到了红霉素肟,产品纯度95.5%,工艺收率97%。研究了p H值、碱、溶剂、盐酸羟胺的量、温度、结晶溶剂等对红霉素肟合成的影响。

Erythromycin thiocyanate was used as raw material,hydroxylamine hydrochloride as oximation reagent,sodium hydride as base,methanol as solvent,to synthesize erythromycin oxime salt,then neutralized by 20% sodium hydroxide,extracted by dichloromethane,obtained the erythromycin oxime by crystallized in 30% methanol in one pot with 95.5% purity and 97% yield of products.The effect of p H value,base,solvent,the amount of hydroxylamine hydrochloride,temperature,crystallization solvent on the synthesis of the target product erythromycin oxime were discussed in this paper.