摘要
利用三异丁基硼氢化锂(L-selectride)试剂还原3-氧代-22-羟基何伯烷得到单一构型的3α,22-二羟基何伯烷和3β,22-二羟基何伯烷.在此基础上,通过X-射线单晶衍射实验确认了3β,22-二羟基何伯烷的绝对构型,并完整归属了该类化合物的^(1)H和^(13)C NMR数据.本文的方法亦可用以制备其他使用常规方法难以分离的α-和β-异构体.
Pure a-and b-isomers of 3,22-dihydroxyhopane were obtained by the reduction of hydroxyl protected hydroxyhopanone with L-selectride.The absolute configuration of 3β,22-hydroxyhopane was confirmed by single crystal X-ray diffraction,and the unambiguous^(1)H and^(13)C NMR data of two isomers were fully assigned for the first time.The preparation method is suitable for the separation of other unseparatedα,β-isomers.
作者
姜垒
付阳
郭文文
郑果
王强
JIANG Lei;FU Yang;GUO Wen-wen;ZHENG Guo;WANG Qiang(High and New Technology Research Center of Henan Academy of Sciences,Zhengzhou 450002,China;Henan Institute of Reproduc tive Health Science and Technology,Zhengzhou 450002,China)
出处
《波谱学杂志》
CAS
北大核心
2021年第2期255-267,共13页
Chinese Journal of Magnetic Resonance
基金
河南省科技攻关计划项目(192102310407)
河南省科学院基本科研经费资助项目(210602006)
河南省医学科技攻关计划项目(LHGJ20190829)
国家卫健委出生缺陷预防重点实验室基本科研经费资助项目(JBKY2020012).