2-(4-氨基-4-甲基戊基)丙二酸二甲酯的合成与表征  

Synthesis and Characterization of Dimethyl 2-(4-Amino-4-methylpentyl)malonate

作　　者：仝红娟 刘斌[1] 赵梅梅 TONG Hong-juan;LIU Bin;ZHAO Meimei(Collaborative Innovation Center of Green Manufacturing Technology for Traditional Chinese Medicine in Shaanxi Province,School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xianyang 712046,China)

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

出　　处：《化学试剂》2021年第9期1286-1290,共5页Chemical Reagents

基　　金：陕西省自然科学基础研究计划项目(2019JQ924);陕西省中药绿色制造技术协同创新中心重点培育项目(2019XT-1-03);陕西省教育厅2020年度专项科学研究计划项目(20JK0510)。

摘　　要：标题化合物是一种新结构的合成7,7-二甲基吖庚环-2-酮的中间体,该文报道其合成方法及表征。以丙烯酸甲酯和2-硝基丙烷为原料,经过Michael加成反应、酯水解反应、缩合反应、羰基还原反应、酯交换反应以及硝基还原反应,合成得到目标化合物。6步反应总产率达到40%。产物及中间体结构经^(1)HNMR、^(13)CNMR、FT-IR、元素分析及MS表征。其中,Michael加成产物4-甲基-4-硝基戊酸的结构进一步通过X-单晶衍射确定。并对每一步反应条件进行了简单讨论。该研究为吖庚环-2-酮类化合物的合成提供了一种新颖的中间体结构。The synthesis and characterization of a novel 7,7-dimethyl azepan-2-one intermediate compound 2-(4-amino-4-methylpentyl)malonate was reported.The target compound was synthesized from methyl acrylate and 2-nitropropane through a six-step reaction in a total yield of 40%,involving Michael addition reaction,hydrolyzation of ester,condensation reaction,carbonyl reduction,transesterification and nitro reduction.The structure of intermediates and the product were characterized by ^(1)HNMR,^(13)CNMR,FT-IR,elemental analysis and MS.The structure of Michael addition product 4-methyl-4-nitropentanoic acid was further determined by X-ray diffraction analysis.Also,the reaction conditions of each step were discussed briefly.This study provides a novel intermediate structure for the synthesis of azepan-2-one derivatives.

关 键 词：吖庚环衍生物 吖庚环-2-酮 X-射线单晶衍射 合成 表征 

分 类 号：TQ463[化学工程—制药化工]