基于固体酸HClO4/SBA-15催化的奥硝唑合成

Synthesis of Ornidazole Based on Solid Acid Catalyst HClO4/SBA -15

摘要:

将分子筛SBA-15负载高氯酸制备了一种固体酸催化剂（HClO4/SBA-15），并利用红外光谱对其进行了表征。开发了以HClO4/SBA-15为催化剂，2-甲基-5-硝基咪唑和环氧氯丙烷为原料的奥硝唑合成方法。考察了不同催化用量、反应时间、反应温度、不同溶剂对转化率的影响。优化反应条件为：催化剂用量为2-甲基-5-硝基咪唑：HClO4/SBA-15等于5:3，异丙醇作溶剂，在0℃下反应8h时，奥硝唑得率高达76.3％，纯度为99.8%。采用核磁共振波谱仪，质谱分析仪对产物进行了鉴定。该方法合成的奥硝唑质量符合药典质量标准。催化剂可重复使用，第三次使用时转化率仍有65.8％。

Abstract:

The solid acid catalyst (HClO4/SBA-15) was prepared by using a molecular sieve SBA-15 supported perchloric acid, and characterized by infrared spectroscopy. A method for the synthesis of ornidazole with solid acid HClO4/SBA-15 as catalyst, 2-methyl-5-nitroimidazole and epichlorohydrin was developed. The influences of different catalytic dosage, reaction time, reaction temperature and different solvents on the conversion were investigated. The optimum conditions showed that when the amount of 2-methyl-5-nitroimidazole: HClO4 / SBA-15 was equal to 5:3, and the reaction was carried out at 0°C for 8h with the reaction of isopropanol as the solvent, the conversion of 2-methyl-5-nitroimidazole could reach to 76.3%, Purity of 99.8%. The product was identified by nuclear magnetic resonance spectroscopy and mass spectrometer. The results showed that the quality of ornidazole was consistent with the quality standard of pharmacopoeia. The catalyst can be reused and the conversion rate is still 65.8% for the third use.