目的合成可用于生物材料表面改性的活性中间体二氯磷酰胆碱。方法由三氯氧磷和氯化胆碱在无水条件下用非均相一步法合成二氯磷酰胆碱,并对合成条件进行了探讨,对产物进行了表征和含量测定。结果产物结构由^31P NMR和IR得到证明,产物含量用改进的电位滴定法进行了测定。在最佳反应条件下,收率可以达到100%,目标产物含量可达91%。结论非均相一步合成二氯磷酰胆碱的方法可行,改进的电位滴定法适用于磷酸酯/盐混合体系的组分分析,对于提高目标产物的产率及改进合成条件均有指导意义。
Aim To synthesize phosphorylcholine dichloride,a useful reactive intermediate,which can be used in surface modification of biomaterials.Methods Phosphorylcholine dichloride was synthesized directly from phosphoryl chloride and choline chloride under anhydrous condition in a single step reaction.The synthetic conditions were studied.The product was characterized by 31P NMR and IR spectra.The content of product was analyzed by a modified potentiometric titration method here.Results The structure of the product was confirmed by 31P NMR and IR spectra.The content can reach 91% with a yield of 100% under the optimum conditions.Conclusion The synthetic method of phosphorylcholine dichloride is feasible.The developed potentionmetric technique is good at analyzing the composition of phosphate mixture,and also helpful for searching for superior synthetic conditions.