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。
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.
出处
《日用化学工业》
CAS
CSCD
北大核心
2014年第3期147-150,共4页
China Surfactant Detergent & Cosmetics
关键词
薄荷基甲酸薄荷酯
合成
感官评价
menthyl menthylformate
synthesis
sensory evaluation
