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.
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)
出处
《中国药物化学杂志》
CAS
CSCD
2022年第4期289-292,共4页
Chinese Journal of Medicinal Chemistry