刺乌头碱氢溴酸盐的合成及晶体结构

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) nm, b＝1.2196(3) nm, c＝1.2282(2) nm, β＝90.87(1)°, V＝1.59037(54) nm³, Z＝2, D_m＝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.

Synthesis and Crystal Structure of Lappaconitine Hydrobromide

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) nm³, Z＝2, D_m＝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.