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作 者:徐缓[1] 于涛[1] 张伟[1] 尹朋朋[1] 邢永恒[1]
机构地区:[1]辽宁师范大学化学化工学院
出 处:《北华大学学报(自然科学版)》2011年第6期656-658,共3页Journal of Beihua University(Natural Science)
基 金:国家自然科学基金项目(81102394)
摘 要:改进AE-活性酯的合成方法,采用亚磷酸三乙酯代替传统的三苯基膦为脱水剂,二氯甲烷和丙酮混合溶剂(1 1,V V)作为反应溶媒,得到的AE-活性酯外观为淡黄色结晶粉末,产率89.55%,熔点130~132℃,纯度99.14%.确定了以冰乙酸为溶剂、结晶紫为指示剂,用高氯酸标准溶液进行滴定检测AE-活性酯纯度的方法.实验建立的方法稳定、可靠,为AE-活性酯的合成和纯度测定提供了参考.To improve the synthetic method of AE-active ester,triethyl phosphate was adopted as the dehydrating agent to replace conventional tripheny phosphine and methylene chloride and acetone mixture(11,VV) was used to the reaction solvent.The appearance of AE-active ester was light yellow crystalline powder.Its yield was 89.55%,melting point was 130~132 ℃,and purity determination was 99.14%.The purity of AE-active ester was determined by the titration method which adopted glacial acetic acid as solvent,perchloric acid as standard solution,crystal violet as indicator.The result indicated that the new synthetic and determined methods have a good stability and reliability.It could provide some references for relevant study on detection and synthesis of AE-active ester.
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