摘要
以环己基甲酸为原料 ,采用新的工艺通过酰氯化、傅—克酰基化反应、卤化、水解制得 1-羟基环己基苯基甲酮光引发剂。新工艺选取三氯化磷为酰氯化剂 ,环己基甲酸与三氯化磷的为酰氯化剂 ,环己基甲酸与三氯化磷的物质的量比为 1∶0 .4 3,75℃下反应 2 .5h ,收率 94 .6 %。卤化反应中采用溴为卤化剂 ,70℃下反应 ,反应时间 0 .2 5h ,收率98%。跟原工艺相比 ,新工艺大大减少了有害气体的产生 ,缩短了反应时间 ,且全程收率达到 6 9%。
The photoinitiator 1-hydroxycyclohexylphenylketone was prepared using cyclohexanecarboxylic acid as raw materials through acyl chloridation,Frield-Crafts reaction,halogenation and hydrolysis.PCl 3 was selected as acyl chloridation agent in the new process and the molar ratio of CCA to PCl 3 was 1∶0.43.The reaction proceeded at 75℃ for 2.5 h.The yield was 94.6%.Bromine was used in halogenation at 70℃ for 0.25 h and the yield was 98%.Compared with the traditional procedure,the method metioned in this article not only reduced the emission of hazardous gas,but also shortened the reaction period.The total yield was 69%.
出处
《化工时刊》
CAS
2004年第8期49-50,共2页
Chemical Industry Times
