玫瑰麝香酯的合成研究  

Synthesis of rosamusk fragrance ester

作　　者：沈德立[1] 穆旻[2] 何昕[1] 刘玉平[1] 田红玉[1] 孙宝国[1] 

机构地区：[1]北京工商大学食品学院食品风味化学北京市重点实验室,北京100048 [2]中国香料香精化妆品工业协会,北京100079

出　　处：《日用化学工业》2014年第9期508-511,共4页China Surfactant Detergent & Cosmetics

基　　金：国家科技部科技支撑计划资助项目(2011BAD23B01)

摘　　要：首先以二氢月桂烯和甲酸为原料、浓硫酸为催化剂,合成了甲酸1-(3,3-二甲基环己基)乙醇酯;然后甲酸1-(3,3-二甲基环己基)乙醇酯在氢氧化钠的甲醇溶液中皂化,得到了1-(3,3-二甲基环己基)乙醇;最后以对甲苯磺酸为催化剂,1-(3,3-二甲基环己基)乙醇与乙酸酐反应合成了玫瑰麝香酯。考察了原料摩尔比、反应时间和反应温度对玫瑰麝香酯产率的影响,并通过红外光谱、气-质联用和核磁共振等对所合成的中间体和目标产物的结构进行了表征,并对合成的玫瑰麝香酯进行了香气评价。结果表明,各步反应中均得到了目标产物;终产物玫瑰麝香酯的收率为91.1%,其具有温和的木香、玫瑰香、果香、甜香,并带有香叶、药草、麝香气息。Firstly, intermediate 1 - （ 3,3 - dimethylcyclohexyl） ethyl formate was prepared with dihydromycene and formic acid as starting materials and concentrate sulfuric acid as catalyst. Then the intermediate was saponified by a methanol solution of sodium hydroxide to obtain 1 - （3,3 - dimethyleyclohexyl） ethanol. The latter was further reacted with acetic anhydride in presence ofp -toluenesulfonic acid as catalyst to prepare the targeted product rosamusk fragrance ester. Influences of mole ratio of materials, reaction time and reaction temperature on yield of the product were investigated in order to optimize the synthetic conditions. The structures of intermediate and product were characterized by means of IR, GC - MS,1HNMR and 13CNMR, while the odor characteristic of the targeted product was evaluated. The results showed that all the designed reaction steps were carried out in order and the yield of the targeted product achieves 91.1%. The odor evaluation result indicated that the targeted product displays a mild wood fragrance, rose fragrance, fragrance, sweet fragrance as well as a flavor of geranium, herb and musk.

关 键 词：香料 玫瑰麝香酯 合成 二氢月桂烯 

分 类 号：TQ655[化学工程—精细化工]