刺乌头碱氢溴酸盐的合成及晶体结构

Synthesis and Crystal Structure of Lappaconitine Hydrobromide

报道了以双溴代烷烃和刺乌头碱合成刺乌头碱氢溴酸盐的方法.用元素分析、红外光谱、高分辨质谱和核磁共振进行了表征.并用X射线单晶衍射确定了标题化合物的绝对构型.晶体结构表明,该化合物通过分子间氢键形成了网状类似超分子结构.晶体属于单斜晶系,P21空间群,晶胞参数:a=1.0619(2)am,b=1.2196(3)nm,c=1.2282(2)nm,β=90.87(1)°,V=1.59037(54)am3,Z=2,Dm=1.428 g/cm-3,F(000)=720.0,μ=1.349 mm-1.环A,B,C,D,E和F分别呈船式、椅式、信封式、船式、船式和信封式.其绝对构型被确定为1S,4S,5S,7S,8S,9S,10S,11S,13R,14S,16S,17R.

A method for the synthesis of lappaconitine hydrobromide by the reaction of dibromoalkyl with lappaconitine is presented. Lappaconitine hydrobromide was determined by IR, 13C NMR, HRMS spectra, elemental analysis and X-ray diffraction analysis. Through intermolecular hydrogen bonding, the similar super molecule netlike structure is formed. Crystal data： monoclinic, P21, a= 1.0619（2） nm, b=1.2196（3） nm, c= 1.2282（2） nm, β=90.87（1）°, V= 1.59037（54） nm^3, Z=2, Dm= 1.428 g/cm^-3, F（000）=720.0, μ= 1.349 mm^-1. Rings A, B, C, D, E and F present boat, chair, envelope, boat, boat and envelope forms, respectively. The stereo absolute configuration of lappaconitine hydrobromide was determined as 1S,4S,5S,7S,8S, 9S,10S,11S,13R,14S,16S,17R.