唑的合成研究  

Synthesis of oxazole

作　　者：唐文强 高艳蓉 仝红娟 王艳娇[1,2] TANG Wen-qiang;GAO Yan-rong;TONG Hong-juan;WANG Yan-jiao(School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xi’an 712046,China;Collaborative Innovation Center of Green Manufacturing Technology for Traditional Chinese Medicine in Shaanxi Province,Xi'an 712046,China)

机构地区：[1]陕西国际商贸学院医药学院,陕西西安712046 [2]陕西省中药绿色制造技术协同创新中心,陕西西安712046

出　　处：《精细与专用化学品》2020年第3期28-31,共4页Fine and Specialty Chemicals

基　　金：陕西省教育厅专项科研计划项目(19JK0101);生物医药创新制药技术研究院士专家工作站资助项目(陕科协发[2017]事企字15号);陕西国际商贸学院中药质量标志物创新团队项目(SSY18TD02)。

摘　　要：以对甲苯磺酰甲基异氰(化合物2)和多聚甲醛为原料,在碱性条件下反应得到4-甲苯磺酰基-4,5-二氢唑(化合物3),化合物3再经强碱性脱除对甲苯磺酰基得到唑(化合物1),产物及中间体结构经1 HNMR和MS确证。确定的化合物3的最佳反应条件为:n(多聚甲醛)∶n(化合物2)=1.05∶1,反应溶剂为二甲基亚砜,n(K2CO3)∶n(化合物2)=1.1∶1,反应时间为5h。在此最佳工艺条件下,化合物3的收率为84.8%。Oxazole was synthesized from TOSMIC and paraformaldehyde through a two-step reaction.Firstly,4-tosyl-45-dihydrooxazole(3)was obtained in basic condition,then oxazole(1)was obtained by TOS group removed also in basic condition.The structure of the product and intermediate were confirmed by 1 HNMR and MS.The effect of reaction conditions on the yield of compound 3 were investigated,the optimal conditions were as follows:the mole ratio of n(paraformaldehyde)∶n(compound 2)=1.05∶1,the solvent is DMSO,the amount of K2 CO3 is n(K2 CO3)∶n(compound 2)=1.1∶1,the reaction was at room temperature for 5 h.Compound 3 was obtained in the yield of 84.8%by optimal reaction conditions.

关 键 词：唑 Van Leusen反应 对甲苯磺酰基异氰 合成 

分 类 号：TQ463[化学工程—制药化工]