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Synthesis of rosamusk fragrance ester
SHEN De-li, MU Min, HE Xin, LIU Yu-ping, TIAN Hong-yu, SUN Bao-guo
2014, 44 (9):
508-511.
doi: 10.13218/j.cnki.csdc.2014.09.114
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-dimethylcyclohexyl) ethanol.The latter was further reacted with acetic anhydride in presence of p-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,fruit fragrance,sweet fragrance as well as a flavor of geranium,herb and musk.
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