从银杏叶中分离制备聚戊烯醇混合物(C75~C10),纯度为87.2%,选择POCl3为磷酰化剂和三乙胺为碱性水解剂,经过磷酰化和水解二步反应,聚戊烯基氯磷酸酯在三乙胺碱性溶液中转化成聚戊烯基磷酸酯,产品得率在65%以上。聚戊烯醇与POCl3的摩尔比为1:5~10,反应温度低于10℃;室温水解20h,反应产物经柱层析纯化和HPLC制备聚戊烯基磷酸酯,由IR、^1H NMR、^13CNMR和高分辨质谱(HRMS)鉴定其化学结构为聚戊烯基单磷酸酯。
Polyprenols( C75 - C110 ) of purity over 87.2 % were separated and prepared from leaves of Gingkgo biloba L. Polyprenyl phosphate dichlorate was synthesized by choosing phosphorus oxychloride ( POCl3 ) as phosphate, and was converted into polyprenyl phosphate with triethanylamide as hydrolytic reagent with yield more than 65 %. The molar ratio of polyprenols to POC13 was 1 : 5 - 10. Phosphate ester reaction temperature was below 10℃, and hydrolysis for 20 h at room temperature. The hydrolysate was purified by silicon gel chromatography and polyprenyl phosphate was obtained by HPLC, and its chemical structure was identified as polyprenyl monophosphate with IR, ^1H NMR,^ 13C NMR and HRMS.