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日用化学工业 ›› 2014, Vol. 44 ›› Issue (3): 147-150.doi: 10.13218/j.cnki.csdc.2014.03.034

• 开发与应用 • 上一篇    下一篇

薄荷基甲酸薄荷酯的合成研究

岳海波1, 梁娅2, 陈义坤1, 戴莉2, 郭春生2, 张峻松2   

  1. 1.湖北中烟工业有限责任公司 烟用植物应用研究行业重点实验室,湖北 武汉 430040;
    2.郑州轻工业学院 食品与生物工程学院,河南 郑州 450002
  • 收稿日期:2013-11-28 发布日期:2019-04-09
  • 作者简介:岳海波(1983-),男,河南新乡人,学士,电话:(027)83603038,E-mail:yhb.1983@163.com。

Synthesis of menthyl menthylformate

YUE Hai-bo1, LIANG Ya2, CHEN Yi-kun1, DAI Li2, GUO Chun-sheng2, ZHANG Jun-song2   

  1. 1.Key Laboratory of Applied Research on Natural Plant for Tobacco,China Tobacco Hubei Industrial Co.,Ltd., Wuhan,Hubei 430040,China;
    2.School of Food and Bioengineering,Zhengzhou University of Light Industry, Zhengzhou,Henan 450002,China
  • Received:2013-11-28 Published:2019-04-09

摘要: 首先以薄荷基甲酸与亚硫酰氯为原料,制得薄荷基甲酰氯;然后以薄荷基甲酰氯和L-薄荷醇进行反应,用无水吡啶为溶剂和缚酸剂,一锅法制得薄荷基甲酸薄荷酯。通过单因素实验和正交试验设计确定优化条件为:n(L-薄荷醇)∶n(薄荷基甲酸)=1∶1.5,n(L-薄荷醇)∶n(无水吡啶)=1∶6,反应温度为60 ℃,搅拌反应3 h,平均收率达83.91%。得到的目标产物经过IR,1HNMR及MS对其结构进行确认,通过感官评价可知薄荷基甲酸薄荷酯具有较好生理凉感,味觉凉感阈值为1.5 mg·L-1,100 mg·L-1的薄荷基甲酸薄荷酯溶液浸渍的滤纸条能在口中维持凉感的持续时间约为20 min。

关键词: 薄荷基甲酸薄荷酯, 合成, 感官评价

Abstract: Firstly,menthyl formic acid and thionyl chloride were used as starting materials to prepare menthyl formyl chloride and then menthyl menthylformate was prepared via the reaction of the menthyl formyl chloride and menthol,with anhydrous pyridine as solvent as well as acid absorbing agent.Single factor tests as well as orthogonal designed tests were carried out and the optimal reaction conditions were identified as:mole ratio of the chemical reagents,n(menthol)∶n(menthyl formic acid)=1∶1.5,n(menthol)∶n(pyridine)=1∶6;reaction temperature,60 ℃ for 3 h.Under such conditions,the average yield achieves 83.91%.Structure of the targeted product was characterized by IR,1HNMR and MS.Via sensory evaluation,the targeted product shows good cool feeling and its threshold value achieves 1.5 mg·L-1.A filter paper strip impregnated with 100 mg·L-1 solution of the targeted product can maintain cool feeling in mouth for 20 min.

Key words: menthyl menthylformate, synthesis, sensory evaluation

中图分类号: 

  • TQ65