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The CTC Direct Hydrolysis of the synthesis of the photoinitiator agent alpha - hydroxy cyclohexyl phenyl ketone and 2 - Hydroxy-2 - methyl-1 - phenyl-1 - propyl ketone ! Using infrared spectroscopy, GC spectrometer and NMR to characterize the structure of the reaction products and intermediates , and the reaction mechanism was discussed . Each of cyclohexyl methyl chloride, and isobutyryl chloride as the raw materials, the use of anhydrous aluminum trichloride as catalyst , cyclohexyl phenyl ketone intermediates and isobutyryl benzene intermediates generated by Friedel-Crafts acylation reaction in benzene . Cyclohexyl phenyl ketone , optimum conditions are: material ratio of n ( cyclohexyl - methyl chloride ) : n ( anhydrous aluminum chloride ) = 1:1.2, n ( cyclohexyl chloride ) : n ( benzene ) = 1:6 , and the reaction temperature for 5-8 ° C , the reaction time was 4h , cyclohexyl phenyl ketone in 91% yield , purity greater than 99% . The isobutyryl benzene optimum conditions : material ratio of n ( iso chloride ) : n ( anhydrous aluminum chloride ) = 1:1.2 , n ( iso chloride ) : n ( benzene ) = 1:3 the reaction temperature is 15 ° C , the reaction time of 5h , isobutyryl benzene , yield 87% , purity of greater than 99% . In aqueous potassium hydroxide solution , adding carbon tetrachloride, tetrabutyl ammonium bromide as a phase transfer catalyst , the the intermediate cyclohexyl phenyl ketone and isobutyryl benzene directly chlorinated then hydrolysis of the alpha - hydroxy- cyclohexyl phenyl- methanone and 2 - hydroxy-2 - methyl-1 - phenyl-1 - propyl ketone . Synthesis of α- hydroxy cyclohexyl phenyl ketone The optimum conditions are: material ratio of N ( cyclohexyl - phenyl ketone ) : n ( potassium hydroxide ) = 1:8 , n ( cyclohexyl phenyl ketone ) : n ( carbon tetrachloride) = 1:2.0 , reaction temperature of 70 ° C , the reaction time was 6h, 96% yield , purity greater than 99% . Synthesis of 2 - hydroxy-2 - methyl-1 - phenyl-1 - propyl ketone optimum conditions : feed ratio the n ( isobutyrylacetate benzene ) : n ( potassium hydroxide ) = 1:8 , n ( isobutyryl benzene ) : n ( carbon tetrachloride) = 1:2.0 , reaction temperature of 70 ° C , the reaction time of 6 h , yield 84% , purity greater than 99% .
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