Study On Synthesis Of Calone

Because of its unique fresh fruit and sea air, calone is now widely used in daily chemical products, its synthesis is more and more significance. In this paper, the main raw materials are 1,3-dichloro acetone and 4-methyl catechol. Calone was synthesized through the nucleophilic addition reaction and cyclization rearrangement reaction, and their process conditions were optimized. This point of view starting from the following two studies:Firstly the nucleophilic addition reaction was investigated. Catalyst which was used in the process, catalyst and 4-methyl-catechol molar ratio,1,3-dichloro acetone and 4-methyl catechol molar ratio, solvent and the dosage on the reaction yield, and later by the orthogonal experimental method to further define the impact of various factors on the degree of yield:Catalyst> Catalyst and 4-methyl-catechol molar ratio> 1,3-dichloro-acetone and 4-methyl catechol molar ratio>solvent. The best reaction conditions of nucleophilic addition reaction:potassium hydroxide as catalyst; catalyst and 4-methyl-catechol molar ratio of 1:0.75; 1,3-chlorine acetone and 4-methyl catechol molar ratio of 1:1.2; methanol as solvent; solvent dosage of 60ml; reaction temperature is 65℃; reaction time was 4 hours.Second, the studies into the rearrangement process:the catalyst, catalyst amount, time effect on the reaction.At last, the optimum conditions in the rearrangement:the potassium carbonate catalyst; intermediate and catalyst mole ratio of 1:2; reaction time was 4 hours.After more than two-step reaction, the final yield of calone 60.21%.The reaction products were identified the structure of its material by GC-MS, NMR analysis...