对硝基苯甲醛-d_5的合成  

Synthesis of deuterium-labelled p-nitrobenzaldehyde-d_5

作　　者：梁大伟[1] 王悦秋[1] 叶群丽[1] LIANG Da-wei;WANG Yue-qiu;YE Qun-li(School of Pharmacy & Medical Laboratory Science,Ya'an Polytechnic College,Ya'an 625000,China)

机构地区：[1]雅安职业技术学院药学与检验学院,四川雅安625000

出　　处：《精细与专用化学品》2019年第1期40-43,共4页Fine and Specialty Chemicals

基　　金：雅安市应用技术研究与开发项目(2017YYJSKF15);雅安职业技术学院院级科研项目(YZY2018ZKA02)

摘　　要：以苯-d6为原料,经过溴代、硝基化、氰基化、水解、还原与氧化等六步反应,高效合成了对硝基苯甲醛-d5,对关键步骤氰基化反应的条件进行了优化。对硝基苯甲醛-d5的结构经13 CNMR、IR与MS表征,总收率为24%(以苯-d6计),化学纯度为99.1%,同位素丰度为98.2%。The p-nitrobenzaldehyde-d5 was synthesized by an efficient route from benzene-d6 though 6steps in a total yield of 24%,involving bromation,nitration,cyanylation,hydrolysis,reduction and oxidation reaction.The reaction conditions of cyanylation were optimized.The structures of intermediates and the product were confirmed by 13 CNMR,IR and MS.The chemical purity of the target compound was 99.1% and its isotopic enrichment of D was 98.2%.

关 键 词：氘代标记 对硝基苯甲醛 合成 

分 类 号：TQ24[化学工程—有机化工]