摘要
采用集自动搅拌、过滤、鼓泡等多重功能于一体的自制多肽固相合成反应器,以对称酸酐法、活化酯法、2,6-二氯苯甲酰氯(DCB)法研究了大位阻氨基酸Fmoc-Arg(Pbf)-OH与Rink Amide-AM树脂的连接反应工艺。探讨了催化体系、溶剂体系、反应时间、反应物配比以及搅拌方式对合成Fmoc-Arg(Pbf)-Rink Amide-AM树脂反应的影响。结果表明,采用活化酯法(DIC/HOBt/DMAP)时连接率最高,最佳反应条件为:在采用N2辅助磁力拌系统,以体积比为1∶1的DMA/DCM为反应溶剂,氨基酸与树脂物质的量的比为3∶1,反应时间为3 h时,连接率高达93%。
The coupling reactions of Fmoc-Arg（ Pbf）-OH and Rink Amide-AM Resin with symmetrical anhydride method,active ester method and 2,6-dichlorobenoyl chloride （DCB） method, respectively, were investigated in a self- designed reactor which congregated the stirring, filtration, and bubbling function together. The effects of reaction strategy, solvent system, reaction time, molar ratio of reactants and stirring method on the yield of condensation reaction were performed. The results indicate that the DIC/HOBt/DMAP strategy is the best method. The optimal reaction conditions are shown as follows：3：1 of molar ratio of the reactants,3 h of reaction time and DMA/DCM （ 1： 1, V/V） as a solvent usinz nitrozen-assisted magnetic stir system. The highest yield of the condensation reaction is 93%.
出处
《现代化工》
CAS
CSCD
北大核心
2012年第2期62-65,共4页
Modern Chemical Industry
基金
江苏省自然科学基金资助项目(BK2006181)
江苏省科技厅资助项目(BE2010196)
江苏高校优势学科建设工程资助项目
南京工业大学博士研究生创新计划(BSCX200910)
