尼泊金甲酯的绿色合成.pdf

试验研究 China Food Additives
尼泊金甲酯的绿色合成
李玉文·”,张琦
(1.青岛农业大学化学与药学院,青岛266109
2.齐鲁师范学院学报编辑部,济南250013)
摘要?采用对羟基苯甲酸与碳酸二甲酯为原料,以硅胶负载高氯酸为催化剂,加热反应制得尼泊金甲
酯,测定所合成的尼泊金甲酯的核磁共振氢谱及熔点并与文献报道值枏比较,从而确证所合成的尼泊金甲酯
的结构。对影响尼泊金甲酯收率的因素(反应物配比、反应温度、反应时间及催化剂用量)进行研究,确定尼泊
金甲酯的适宜合成条件:n(碳酸二甲酯):n(对羟基苯甲酸)=2:1,反应温度为90℃,反应时间为8h,催
化剂用量为碳酸二甲酯摩尔量的0.2%,在此条件下尼泊金甲酯的收率达93.1%。与目前合成尼泊金甲酯的
方法相比,该法收率高,硅胶负载高氯酸催化剂可以回收利用,无三废排放,绿色环保,适宜规模化生产。
关键词?尼泊金甲酯:碳酸二甲酯:绿色合成硅胶负载高氯酸
中图分类号:TQ655文献标识码
文章编号:1006-2513(2014)09-0071-03
Green synthesis of methyl paraben
LI Yu-wen, ZHANG Qi
1. College of Pharmacy and Chemistry, Qingdao Agricultural University, Qingdao 266109
2. The Editorial Office, Qilu Normal University, Jinan 250013)
bstract Methyl paraben was prepared by reaction of p-hydroxyl benzoic acid with dimethyl carbonate using HCIO
Sio as catalyst. The structure of methyl paraben was confirmed by measuring and comparing melting p
HMR reported in literature. The actors influencing the yield of methyl paraben was also studied, including reaction
temperature, reactants mole ratio, reaction time and catalyst amount. The best reaction conditions were optimized as
follows the mole ratio of dimethyl carbonate to p-hydroxyl benzoic acid was 2: 1, the reaction temperature wa
90, reaction time was 8h and the catalvst amount was 0. 2%(based on imethy carbonate molar amount
ised on
these conditions, the yield of methyl paraben can be up to 93. 1%o. The advantage of this green synthetic pr
clude high yield, easy recovery and recyclability of dimethy carbonate, no pollution, feasible to apply in industry
Key words. methyl paraben, dimethyl carbonate, green synthesis, HCIO, -Sio2
尼泊金甲酯,又名对羟基苯甲酸甲酯,是
泊金甲酯的经典合成方法是以对羟基苯甲酸和甲
类低毒、无刺激性且适用pH范围较宽的防腐剂,醇为原料,在各种酸性催化剂的作用下制备,所
因而在食品、化妆品及医药领域获得广泛应用。用的催化剂包括?硫酸、对甲苯磺酸、固体超强
因此,研究尼泊金甲酯的合成具有重要意义。尼酸、杂多酸,除浓硫酸外,这些酸性催化剂
收稿日期:2014-08-10
通讯作者
基金项目:基金项目:国家自然科学基金(No.21272131),山东省自然科学基金(No."R2011BIO03),
青岛农业大学博士基金(No.630708)
作者简介:李玉文(1969-),男,副教授,研究方向为药物化学
2014年第9期
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