摘要
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.
出处
《林产化学与工业》
EI
CAS
CSCD
2006年第1期23-27,共5页
Chemistry and Industry of Forest Products
基金
国家自然科学基金资助项目(30170755)
关键词
银杏叶
聚戊烯醇
聚戊烯基磷酸酯
leaves of Ginkgo biloba L.
polyprenol
polyprenyl phosphate
