硅胶负载H_6PMo_9V_3O_(40)催化制备5-硝基水杨酸甲酯  

Synthesis of Methyl 5-Nitrosalicylate Catalyzed by H_6PMo_9V_3O_(40) Supported on Silica Gel

作　　者：吴锦明[1] 沈爱宝[1] 

机构地区：[1]南通大学化学化工学院,江苏南通226001

出　　处：《精细化工》2011年第6期603-605,共3页Fine Chemicals

基　　金：南通市科技计划项目(K2010021);南通大学自然科学基金项目(10Z013)~~

摘　　要：采用硅胶负载Keggin型H6PMo9V3O40催化水杨酸甲酯与硝酸反应制备5-硝基水杨酸甲酯,考察了反应时间、反应温度、催化剂用量、硝酸用量对反应的影响。较佳的反应条件为:四氯化碳为溶剂,m(水杨酸甲酯)∶m(质量分数65%硝酸)∶m(催化剂)=3.04∶3.00∶3.00,45℃反应3 h,5-硝基水杨酸甲酯的产率81.5%,3-硝基水杨酸甲酯的产率12.4%,总产率93.9%;催化剂回收容易,且重复使用5次后,活性基本不变。Methyl 5-nitrosalicylate was synthesized by the nitration of methyl salicylate with nitric acid catalyzed by H6PMo9V3O40 supported on silica gel.The effects of reaction time,temperature,amounts of catalyst and nitric acid on the reaction results were investigated.Under the optimal conditions：m（methyl salicyate）∶ m（mass fraction 65%HNO3）∶ m（catalyst）=3.04∶ 3.00∶ 3.00,in CCl4 at 45 ℃ for 3 h,the yields of methyl 5-nitrosalicylate and methyl 3-nitrosalicylate were 81.5% and 12.4% respectively.The catalyst could be recovered easily and reused for five times without noticeable drop in activity.

关 键 词：5-硝基水杨酸甲酯 硅胶负载H6PMo9V3O40 硝化反应 精细化工中间体 

分 类 号：O625.61[理学—有机化学] O643.36[理学—化学]