Dissertation > Industrial Technology > Chemical Industry > Spices and cosmetics industries > Synthetic perfume

Synthesis of Galaxolide

Author ZhuBiZuo
Tutor TanShiYu
School Chongqing University
Course Chemical Engineering and Technology
Keywords Galaxolide Synthesis α- methyl styrene Tert-amyl alcohol
Type Master's thesis
Year 2009
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Galaxolide is a polycyclic musk , aroma , delicate, very close to the macrocyclic musk nuances , and the physical and chemical properties of stability , the price is relatively inexpensive , can be widely used in perfumes, fragrances , cosmetics, food, medicine and other fields, is a promising synthetic musk varieties. In this paper, α- methyl styrene (AMS), tert-amyl alcohol , propylene oxide, paraformaldehyde as raw materials, three-step synthesis Galaxolide : first AMS and t-amyl alcohol under acidic condensation catalyst, the reaction conditions , the resulting product pentamethyl indane and propylene hydroxyisopropyl reaction occurs , the resulting hexamethyl indan alcohol and then with formaldehyde polymer half aldol condensation reaction , condensation cyclization final product. Each step product by IR, UV-Vis characterization verification. In the synthesis of indane experiments discussed by single factor experiment type and amount of catalyst , reaction temperature, reaction time, materials and other reactions than the impact of factors on the synthesis reaction ; optimized by orthogonal experimental conditions : When n (AMS) : n (H3PO4): n ( tert-amyl alcohol ): n (H2O) = 1.00:0.85:1.15:0.85, at 35 ℃ reaction 6h. Yield up to 59.7% . Indanol in the synthesis , through the single factor experiments discussed kind and amount of solvent , the reaction mass ratio, amount of catalyst, reaction temperature , reaction time and reaction of synthesis of factors ; optimized by orthogonal test conditions: when n (CH2Cl2): n ( indan ): n ( propylene oxide ): n (AlCl3) = 10:0.93:1.00:0.87, at -20 ~ -15 ℃ loop response 5h. Yield up to 62.7% . Finally the synthesis galaxolide , by single-factor experiments discussed type and amount of catalyst , polyoxymethylene , reaction temperature , reaction time and reaction time base cyclization synthesis of factors ; optimized by orthogonal test conditions : When n (CH2Cl2): n ( indanol ): n ( formaldehyde ): n (PCl5): n (H2O) = 2.90:1.00:1.32:0.95:9.5, reacted at 40 ℃ 6h, 60min base cyclization . Yield up to 98.2%. The process chosen more reasonable catalyst and solvent , improving the existing process , reduce the \

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