[1]潘陈新,杨利民,吕金萍.乙烷-1, 1, 2-三羧酸三乙酯的合成工艺优化[J].常州大学学报(自然科学版),2014,(04):19-22.[doi:10.3969/j.issn.2095-0411.2014.04.005]
　PAN Chen-xin,YANG Li-min,LYU Jin-ping.Optimization of Synthetic Process of Triethyl 1, 1, 2-Ethanetricarboxylate[J].Journal of Changzhou University(Natural Science Edition),2014,(04):19-22.[doi:10.3969/j.issn.2095-0411.2014.04.005]
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乙烷-1, 1, 2-三羧酸三乙酯的合成工艺优化()
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常州大学学报(自然科学版)[ISSN:2095-0411/CN:32-1822/N]

卷:
期数:
2014年04期
页码:
19-22
栏目:
化学化工
出版日期:
2014-08-31

文章信息/Info

Title:
Optimization of Synthetic Process of Triethyl 1, 1, 2-Ethanetricarboxylate
作者:
潘陈新; 杨利民; 吕金萍
常州大学 石油化工学院,江苏 常州 213164
Author(s):
PAN Chen-xin;  YANG Li-min; LYU Jin-ping
School of Petrochemical Technology,Changzhou University,Changzhou 213164,China
关键词:
丙二酸二乙酯;  氢化钠;  N;  N-二甲基甲酰胺;  乙烷-1;  1;  2-三羧酸三乙酯
Keywords:
diethyl malonate;  sodium hydride;  N;  N-dimethyl formamide;  triethyl 1;  1;  2-ethanetricarboxylate
分类号:
TQ 460.31
DOI:
10.3969/j.issn.2095-0411.2014.04.005
文献标志码:
A
摘要:
以丙二酸二乙酯为原料,在强碱的作用下与氯乙酸乙酯反应得到乙烷-1, 1, 2-三羧酸三乙酯。采用新的非质子性溶剂N, N-二甲基甲酰胺,通过单因素实验,研究了反应条件对产物收率的影响。发现氢化钠为碱时收率最高,故在氢化钠为碱时,进一步通过正交实验,优化了反应工艺条件。得到的最优条件为投料比n(丙二酸二乙酯): n(氢化钠): n(氯乙酸乙酯)=1.4:1: 1,反应温度为40 ℃,时间为8 h,氯乙酸乙酯的滴加时间为45 min,在该条件下产品收率达到83.3%。产物用IR和1H NMR进行了表征。
Abstract:
Triethyl 1, 1, 2-ethanetricarboxylate was synthesized with diethyl malonate and ethyl chloroacetate in the presence of strong alkali. The new aprotic solvent N, N-dimethyl formamide was employed. A single factor experiment was conducted to investigate the influence of reaction conditions on the product yield. Using sodium hydroxide as alkali, the reaction conditions were further optimized using the orthogonal experiment. The optimal reaction conditions were molar ratios of diethyl malonate to sodium hydride and to ethyl chloroacetate at 1.4:1:1, with reaction temperature at 40 ℃, reaction time for 8 h, and the dropping duration of ethyl chloride for 45 min. Under the optimal conditions, the product yield was 83.3%. The product was characterized by IR and 1H NMR.

参考文献/References:

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备注/Memo

备注/Memo:
作者简介:潘陈新(1988-),男,江苏泗洪人,硕士生。通讯联系人:杨利民(1962-),E-mail:lyang@cczu.edu.cn
更新日期/Last Update: 2014-12-20