氟哌酸锌合成工艺的研究

Study on the synthetic process of zinc norfloxacine

目的 研究氟哌酸锌的合成方法、工艺及结构。方法 采用正交法研究氟哌酸锌的合成方法、最佳工艺 ;应用红外、紫外及热重量分析进行结构分析。结果 用氟哌酸经过两步法合成可得到氟哌酸锌 ;通过红外光谱图确证 :氟哌酸在 1731cm-1处有羧酸的特征吸收峰 ,而氟哌酸锌的红外光谱图 1731cm-1吸收峰消失 ,出现 15 74cm-1吸收峰和 1393cm-1吸收峰 ;说明氟哌酸锌中羧酸的盐类因形成羧酸根负离子 ,使负电荷平均化。由紫外光谱可知 ,氟哌酸在 2 77nm处有最大吸收 ,而氟哌酸锌在2 76nm处有最大吸收 ,与氟哌酸基本一致。通过热重量分析 ,氟哌酸锌含有 7 90 8%的缔合水 ,其起始分解温度为 2 6 1 31℃。结论 采用两步法合成氟哌酸锌可以避免氢氧化钠与硫酸锌的反应 ,使产品质量得以提高。最佳工艺为 :氟哌酸钠合成的最佳工艺是 :氟哌酸与氢氧化钠的摩尔比为 1∶1 1,反应温度为 6 0℃ ;反应时间为 0 5h。氟哌酸锌合成的最佳工艺是 :氟哌酸钠与硫酸锌的摩尔比为 1∶1 1,反应温度为 70℃ ;反应时间为 2h。通过热重量分析 ,表明氟哌酸锌分子中含有

AIM To stndy on the synthetic method, the synthetic process and the structure of zine norfloxacine. METHODS The synthetic method and the optimal process was studied by orthogonal test. The structure was detected by infrared spectrophotometry, UV spetrophotometry and thermogravimetry. RESULT Zinc Norfloxacine was synthesized from norfloxacine and zine sulphate by two steps.The chemical structnre was confirmed by infrared spectrophotometry,The specific absorb peak of carboxyl was 1 574 cm -1 and 1393 cm -1 in infrared spectrogram of zinc noifloxacime. However the specific absorb peak of carboxyl was 1 731 cm -1 in infrared spectrogram of norfloxacine. It showal that carboxylic saline in the molecule of zine norfloxacine mabes negative electric charge average distribntion as carboxglic saline forms carboxylic radicel. The UV spectrogram showed that maxium absorb wave length of norfloxacine was 277 nm and maxinm absorb wave length of zine norflaxcine was 276 nm. It was proved that using thermogravimetry Zine norfloxacine contained 7 908% association water, the initial temperatnre of decomposition was 261 31. ard the molecule of Zinc norfloxacine contained threc molecules of crystal water. CONDNSION In synthetic process of Znie norfloxacine being avoided the reactian between sodium hydrate and Zinc sulphete by the two steps,the quality of production was raised. The optimal synthetic process of sdium norfoxacine is that molar ratio of norfloxcaine to sodium hydrate is 1∶1 1, the reaetion temperatirre is at 60 and reaction time is for 0 5 hour. The optimai synthetic process of Zinc Norfloxacine is that molar ratio of sodium Norfloxcaine to Zinc sulphate is 1∶1 1, reaction temperature is at 70 and reaction time is for 2 hours.