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机构地区:[1]江南大学化学与材料工程学院食品胶体与生物技术教育部重点实验室,江苏无锡214122
出 处:《精细化工》2013年第8期911-914,共4页Fine Chemicals
基 金:国家自然科学基金资助项目(21411004);国家"十一五"重点科技支撑计划项目(2007BAE52B01)~~
摘 要:以α-氯代十二酸(CDA)和氨水为原料,通过氨解反应合成了α-氨基十二酸(ADA),用FTIR、ESI-MS和1HNMR对产物ADA进行结构表征。实验考察了反应温度、反应时间、催化剂用量和投料比等因素对ADA产率的影响,在优化条件下ADA的产率达到81%。温度较高时,CDA水解副反应与氨解主反应竞争使得ADA的产率偏低,据此设计程序升温工艺,在n(NH3)∶n(CDA)=20∶1,70℃下反应12 h然后在100℃下反应4 h,ADA的产率可提高到91%。α-Amino dodecanoic acid(ADA) was synthesized by the amination of α-chloro dodecanoic acid(CDA) and the molecular structure of ADA was identified by FTIR, ESI-MS and ^1HNMR. The effects of reaction temperature, reaction time, dosage of catalyst and ratio of raw materials on the yield of ADA were investigated. The yield of ADA was 81% under the optimum conditions which was accounted as the competition of the side hydrolysis reaction at high temperature. Based on the optimization of reaction conditions, a temperature programming was applied and the yield of ADA achieved 91% under the optimal temperature programming technology when the amination proceeded at 70 ℃ for 12 h and then at 100 ℃ for4 h with n( ammonia) :n( CDA) =20:1.
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