酸催化合成ω - 吖啶戊酸的工艺条件优化

doi:10.3969/j.issn.1006-396X.2014.06.005

石油化工高等学校学报 ›› 2014, Vol. 27 ›› Issue (6): 20-23.DOI: 10.3969/j.issn.1006-396X.2014.06.005

酸催化合成ω - 吖啶戊酸的工艺条件优化

宫哲, 王德慧, 宋官龙, 赵德智

( 辽宁石油化工大学, 辽宁抚顺1 1 3 0 0 1)

收稿日期:2014-10-21 修回日期:2014-11-12 出版日期:2014-12-25 发布日期:2014-12-19
通讯作者: 王德慧( 1 9 8 1 - ) , 男, 博士, 讲师, 从事重质油加工研究; E - m a i l : d h u i w a n g@a l i y u n. c o m。
作者简介:宫哲( 1 9 8 9 - ) , 女, 硕士研究生, 从事精细化工工艺研究; E - m a i l : 3 6 1 8 0 8 8 8 6@q q. c o m。
基金资助:
辽宁省科技厅博士科研启动基金计划( 2 0 1 3 1 0 6 3) ; 辽宁省教育厅科学研究一般项目( L 2 0 1 2 1 3 3) 。

Optimization of the Synthesis of 5(Acridin9yl) Pentanoic Acid Catalyzed by Acid Catalysts

(Liaoning Shihua University，Fushun Liaoning 113001，China)

Received:2014-10-21 Revised:2014-11-12 Published:2014-12-25 Online:2014-12-19

摘要/Abstract

摘要： 在路易斯酸和质子酸既作为催化剂又作为溶剂的条件下, 二苯胺与己二酸通过酸催化环合反应生成 ω - 吖啶戊酸。分别考察了常见催化剂、反应时间、反应温度、催化剂用量、底物投料比等因素对最终产品收率的影响。实验结果表明, HF活性较高、反应时间6h、反应温度6 0℃、 n( 催化剂) / n( 底物) =3、 n( 二苯胺) / n( 己二酸) =1∶3 时, 其产品ω - 吖啶戊酸最高收率达到8 2. 6%。通过 NMR、 MS和元素分析对产品ω - 吖啶戊酸进行表征, 结果表明产物为ω - 吖啶戊酸。HF作为催化剂使得反应温度低、产品易于分离精制、产品纯度较高。

关键词: &omega, - 吖啶戊酸, 催化反应, 路易斯酸, 质子酸

Abstract: 5(acridin9yl)pentanoic acid was prepared using Nphenylaniline and adipic acid as raw materials by cyclization reaction. Lewis acid and Bronsted acid were chosen as catalysts under the condition of solventfree. The effect of sort of catalysts, reaction time, reaction temperature, the amount of catalysts and the mole ratio of reactants on the yields of final products were investigated. The results showed that the yeild of 5(acridin9yl) pentanoic acid can reach 82.6% under the following experimental conditions:HF with high catalytic activity, the reaction time 6 h, the reaction temperature 60 ℃, 3 times molar ratio of the amount of catalyst to substrate, molar ratio of Nphenylaniline to adipic 1∶3. NMR, MS and elemental analysis were used to characterize the product of 5(acridin9yl) pentanoic acid. The temperature of reaction with HF catalyst was low. The product can be easily seperated and purified with high purity. 

Key words: 5(Acridin9yl)pentanoic acid, , Catalytic reaction, , Lewis acid, , Bronsted acid

宫哲, 王德慧, 宋官龙, 赵德智. 酸催化合成ω - 吖啶戊酸的工艺条件优化[J]. 石油化工高等学校学报, 2014, 27(6): 20-23.

Gong Zhe, Wang Dehui， Song Guanlong, Zhao Dezhi. Optimization of the Synthesis of 5(Acridin9yl) Pentanoic Acid Catalyzed by Acid Catalysts[J]. Journal of Petrochemical Universities, 2014, 27(6): 20-23.

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酸催化合成ω - 吖啶戊酸的工艺条件优化

Optimization of the Synthesis of 5(Acridin9yl) Pentanoic Acid Catalyzed by Acid Catalysts

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