调节pH纯化磺胺间甲氧嘧啶的工艺探讨

Discussion on the Process of Adjusting p H to Purify Sulfamonomethoxine

磺胺间甲氧嘧啶是一种人工合成、在兽医临床上使用最广泛的高效抗菌药之一。某公司磺胺间甲氧嘧啶生产线所得产品含量为74%~76%,常规手段纯化困难。磺胺间甲氧嘧啶结构含有伯氨基、磺酰胺基团,表现出酸碱两性,利用碱溶酸沉法通过调节反应溶液的pH,改变磺胺间甲氧嘧啶在水溶液中溶解度(存在状态),将反应杂质与磺胺间甲氧嘧啶分离,达到纯化的目的。实验结果显示:磺胺间甲氧嘧啶的产率与介质溶液的pH密切相关,在8.0~10.0区间内随pH的升高而增大,但纯度则相反。在pH=8.5~9.0范围进行调节,可以得到纯度在95%以上且产率满意的结果。

Sulfamonomethoxine is an artificially synthesized and one of the most widely used high-efficiency antibacterial drugs in veterinary clinics.The product content of the sulfamonomethoxine production line of a certain company is 74%to 76%,which is difficult to purify by conventional means.The structure of sulfamethoxine contains primary amino groups and sulfonamide groups,which exhibits acid-base amphoteric.The pH of the reaction solution is adjusted by alkali-dissolved acid precipitation method to change the solubility(existing state)of sulfamethoxine in aqueous solution.The reaction impurities are separated from the sulfamonomethoxine to achieve the purpose of purification.The experimental results show that the yield of sulfamonomethoxine is closely related to the pH of the medium solution and increases with the increase of pH in the interval of pH=8.0~10.0,but the purity is opposite.In the range of pH=8.5~9.0,the purity above 95%and a satisfactory yield can be obtained.