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作 者:王成章[1] 郑光耀[1] 高彩霞[1] 张思访[1] 曹志庆[1] 沈兆邦[1]
机构地区:[1]中国林业科学研究院林产化学工业研究所,江苏南京210042
出 处:《林产化学与工业》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)
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.
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