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

Study on Synthesis of Calone

Author QiaoChengLi
Tutor ZhengJiaMing
School Tianjin University
Course Chemical processes
Keywords Watermelon ketone Dieckmann condensation Hydrolysis decarboxylation Sodium sand
CLC TQ655
Type Master's thesis
Year 2009
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Watermelon ketone as a flavors and fragrances , is now widely used in cosmetics, food , and therefore its study of the synthesis process is of great significance . Used herein, 4 - methyl catechol diacetate ester as raw materials, two-step reaction synthesis by Dieckmann condensation and hydrolysis decarboxylation one watermelon , and optimize their respective process conditions , various factors affect Dieckmann condensation and hydrolysis decarboxylation reaction studied. This study can be roughly divided into the following two parts: the investigated Dieckmann condensation reaction catalyst type , amount of catalyst, the amount of sodium sand methanol , solvents , and other single factor changes the reaction effect and by orthogonal experiment the method of determining the influence of various factors on the reaction yield significant order , descending , respectively: a catalyst , a catalyst with the raw material 4 - methyl catechol diacetate methyl ester in molar ratio, reaction solvent, reaction temperature . Optimum conditions: Dieckmann condensation reaction of sand with sodium as the catalyst; amount of sodium sand with the raw material molar ratio is 2:1 ; sodium sand in the amount of methanol with the raw material molar ratio is 0.75 ; toluene as solvent, the solvent is used in an amount of 70mL ; reaction temperature 60 ℃; reaction time was 4 hours , Dieckmann, a condensation reaction product of 7 - methyl-3 ,4 - dihydro -2H - 2- methoxy - carbonyl - 1 ,5 - benzo dioxa the Zhuo -3 - ketone closing rate up to 68.77% . Investigated the hydrolysis decarboxylation during the reaction , type of catalyst , amount of catalyst , temperature and other factors change the impact of the reaction effect , determine the optimum conditions of the hydrolysis decarboxylation reaction : 6 mol / L hydrochloric acid and acetic acid as catalyst ; catalyst with reactants a molar ratio of 5:1; reaction time of 8 hours ; reaction temperature 80 ° C , hydrolysis decarboxylation reaction yield of 83.35% . Dieckmann condensation and hydrolysis decarboxylation two-step reaction , one watermelon final yield of 57.32% . Ultimately Dieckmann condensation and hydrolysis decarboxylation reaction products IR, GC-MS , NMR analysis identified the structure of matter .

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