摘要
以N,N-二甲基乙醇胺与月桂酸为原料,对甲苯磺酸作催化剂,合成了月桂酸乙酯基二甲基叔胺中间体,继而与氯乙酸钠反应制得标题化合物。中间体合成的正交实验优化条件为:n(N,N-二甲基乙醇胺)∶n(月桂酸)=1.6∶1;催化剂用量为反应物总质量的1.5%;170℃反应12 h,最高产率>85%。最终产品合成的均匀实验优化结果:异丙醇为溶剂,n(中间体)∶n(氯乙酸钠)=1∶2.2,90℃反应21 h,中间体转化率>98%。得到的标题化合物经丙酮重结晶提纯,HPLC法分析其质量分数>99%,使用FT-IR、ESI-MS1、HNMR进行了结构表征。
A novel betaine surfactant containing ester bond was synthesized through reactions between sodium chloroacetate and the intermediate lauroylethyl dimethyl tertiary amine,which was prepared using lauric acid and N,N-dimethyl ethanolamine as starting materials,p-toluenesulfonic acid as catalyst.The optimum reaction conditions for the intermediate were obtained via the orthogonal experiments：N,N-dimethyl ethanolamine and lauric acid in a molar ratio of 1.6∶1 reacted at 170 ℃ for 12 h,catalyst amount used 1.5%.The maximum yield is above 85%.The uniform experiment showed that the conversion rate of the second step is above 98%,which was undertaken through the reaction of the intermediate and sodium chloroacetate in a molar ratio 1∶2.2,at 90 ℃ for 21 h,isopropyl alcohol as solvent.The final product was recrystaled with acetone.HPLC showed the purity of the lauroylethyl betaine is beyond 99%.The product was confirmed by FT-IR、ESI-MS and 1HNMR spectrometry.
出处
《化学试剂》
CAS
CSCD
北大核心
2011年第5期448-450,共3页
Chemical Reagents
关键词
甜菜碱
表面活性剂
合成
表征
性能
betaine
surfactant
synthesis
characterization
property
