α-羟基环己基苯基甲酮的合成

a-羟基环己基苯基甲酮是一种新型高效光敏引发剂。第一步由环己基甲酸与氯化亚砜合成环己基甲酰氯,当n(环己基甲酸)/n(氯化亚砜)=1:1.4,回流时间为3.5h时,环己基甲酰氯产率为91.7%;第二步以无水三氯化铝为催化剂,用苯与环己基甲酰氯反应合成了环己基苯基甲酮,当催化剂用量为24g,回流时间为3.5h时,产率为88.67%;第三步在氢氧化钠水溶液中,以四氯化碳为氯化试剂,新洁而灭为相转移催化剂,将环己基苯基甲酮经氯代和水解制得a-羟基环己基苯基甲酮。当反应温度60℃,反应时间5h,新洁尔灭用量50mL,四氯化碳用量12mL时,产率为67%。

SYNTHESIS OF α-HYDROXYCYCLOHEXYL PHENYL KETONE

a-Hydroxycyclohexyl phenyl ketone, one of the new-type high-efficient photosensitive initiator, was synthesized through 3 steps: firstly, cyclohexyl carbonyl chloride was prepared from cyclo-hexane carboxylic acid and thionyl chloride, and when n (cyclohexane carboxylic acid) : n(thionyl chloride) was 1 : 1. 4, and reaction time was 3. 5%, the yield of cyclohexyl carbonyl chloride was 91. 7%; secondly, cyclohexyl phenyl ketone was synthesized from benzene and the above mentioned cyclohexyl carbonyl chloride in the presence of anhydrous aluminium trichloride as catalyst, and when the amount of catalyst was 24 g, reaction time was 3. 5 h, the yield of cyclohexyl phenyl ketone was 88. 67%; finally, a - hydroxycyclohexyl phenyl ketone was prepared from cyclohexyl phenyl ketone by chlorination and hydrolysis in the presence of NaOH(aq), CCl4 and benzalkonium bromide as phase transfer catalyst, and when reaction temperature was 60 ℃, reaction time was 5 h, benzalkonium bromide was 50 mL and CCl4 was 12 mL, the yield of the product could be up to 67%. Elemental analysis, IR and 1H NMR were used to characterize the structure of the product.