基于固体酸HClO4/SBA-15催化的奥硝唑合成  

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

作　　者：陈灿 龚福春[1] 夏姣云[1] 陈雪娇 邹武 CHEN Can, GONG Fu-chun , XIA Jiao-yun, CHEN Xue-jiao, ZOU Wu(School of Chemistry and Biologic Engineering, Changsha University of Science and Technology, Changsha 410004 Hunan , Chin)

机构地区：[1]长沙理工大学化学与生物工程学院

出　　处：《精细化工》2018年第4期716-720,共5页Fine Chemicals

基　　金：国家自然科学基金(11405013);中科院上海有机所生命有机化学国家重点实验室开放基金(SKLBNPC12423)~~

摘　　要：将分子筛SBA-15上负载高氯酸,制备了一种固体酸催化剂（HCl O4/SBA-15）,利用IR对其结构进行了表征。并以HCl O4/SBA-15为催化剂,2-甲基-5-硝基咪唑和环氧氯丙烷为原料合成了奥硝唑,考察了催化用量、反应时间、反应温度、不同溶剂对产物收率的影响。得到优化的反应条件为：催化剂质量分数为60%（以2-甲基-5-硝基咪唑的质量为基准,下同）,异丙醇作溶剂,在0℃下反应8 h,奥硝唑收率达76.3%,纯度（HPLC）为99.8%。采用1HNMR、^13CNMR和MS确认产物结构。该法合成的奥硝唑质量符合药典质量标准。催化剂重复使用3次后,产品收率仍能达到65.8%。A solid acid catalyst（HCl O4/SBA-15） was prepared by introducing perchloric acid into molecular sieve SBA-15 and characterized by means of IR. A method for the synthesis of ornidazole using solid acid HCl O4/SBA-15 as catalyst and 2-methyl-5-nitroimidazole and epichlorohydrin as reactants was developed. The influences of catalytic dosage,reaction time,reaction temperature and different solvents on the yield of product were investigated. The optimum conditions were obtained.When the amount of catalyst was 60% of the mass of 2-methyl-5-nitroimidazole and the reaction was carried out at 0 ℃ for 8 h with isopropanol as the solvent,ornidazole in a yield of 76. 3% could be obtained with a purity of 99. 8%（HPLC）. The product was identified by1 HNMR,^13 CNMR and MS.The results showed that the quality of the synthesized ornidazole was consistent with the quality standard of pharmacopoeia. In addition,the yield of product could still reach 65. 8% after it was repeatedly used for three times.

关 键 词：固体酸催化剂 奥硝唑 HClO4/SBA-15 精细化工中间体 

分 类 号：TQ612[化学工程—精细化工]