4,4-(二甲基环己烯-1-基)硼酸频哪醇酯的合成工艺研究  

Study on the synthetic process of 4,4-dimethylcyclohexen-1-boronic acid pinacol ester

作　　者：丁志新 李成斌 李成利 门靖 田真真 郭洁芬 DING Zhi-xin;LI Cheng-bin;LI Cheng-li;MEN Jing;TIAN Zhen-zhen;GUO Jie-fen(Xi′an Wanlong Pharmaceutical Co.,Ltd.,Xi'an 710119,China)

机构地区：[1]西安万隆制药股份有限公司,陕西西安710119

出　　处：《中国药物化学杂志》2022年第4期289-292,共4页Chinese Journal of Medicinal Chemistry

摘　　要：目的优化4,4-(二甲基环己烯-1-基)硼酸频哪醇酯的合成工艺。方法以丁烯酮和异丁醛为起始原料,经缩合、氢化、溴代、硼酸化和缩合反应得到4,4-(二甲基环己烯-1-基)硼酸频哪醇酯。结果与结论目标产物及部分中间体的结构经MS、^(1)H-NMR确证,总收率为19.6%(以丁烯酮计),纯度为99.6%(GC法)。该合成方法所得产品纯度较高,成本相对较低,具有市场竞争力。An improved synthetic process of 4,4-dimethylcyclohexen-1-boronic acid pinacol ester was reported.4,4-Dimethylcyclohexen-1-boronic acid pinacol ester was synthesized via condensation,hydrogenation,bromination,converting to boronic acid and condensation with pinacol.The structures of the target product and intermediates were confirmed by MS and~1H-NMR.The overall yield was up to 19.6%(based on methyl vinyl ketone)with the GC purity of 99.6%.The improved process has the advantages of inexpensive materials and high purity.

关 键 词：4 4-(二甲基环己烯-1-基)硼酸频哪醇酯 edicotinib 合成工艺 

分 类 号：R914[医药卫生—药物化学]