摘要
苦皮藤根皮粉经苯回流提取、大孔树脂层析和硅胶层析后获得苦皮藤素Ⅴ。以正丙醇和苦皮藤素Ⅴ为原料,建立了基于无水碘代反应和威廉姆逊反应的6β-丙氧基苦皮藤素Ⅴ的微量合成方法,反应总收率约为17%。最终产物以HRMS、1H NMR和13C NMR确认为6β-丙氧基苦皮藤素Ⅴ。HPLC分析表明,该产物纯度大于98%。该方法为杀虫活性成分6β-丙氧基苦皮藤素Ⅴ的放射性同位素标记合成奠定了基础。
An insecticidal compound 6β-propoxycelangulin V was synthesized from celangulin V and 1-propanol through anhydrous iodination and Williamson reactions. The purpose of the study was to develop the microsynthetic method of 6β- propoxycelangulin V. The powdered root bark of Chinese bittersweet ( Celastrus angulatus Max. ) was extracted by benzene under reflux, followed by purification by macroporous-resin and silica-gel chromatography. The desired product was purified by RP-HPLC and identified by HRMS, ^1H NMR and 13^ C NMR. The total yield was about 17 %, and the purity was higher than 98%. This method could be applied in radiosythesis of 6β-( [ 1-^14C]propoxy)celangulin V.
出处
《核农学报》
CAS
CSCD
北大核心
2008年第2期223-227,共5页
Journal of Nuclear Agricultural Sciences
基金
国家自然科学基金(30130130)
973项目(2003CB114404)