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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。
The reaction of methyl salicylate with nitric acid catalyzed by Keggin-type H6PMo9V3O40 on silica gel was carried out to prepare methyl 5-nitrosalicylate. The effects of reaction time, reaction temperature, catalyst dosage and nitric acid dosage on the reaction were investigated. The preferred reaction conditions are as follows: carbon tetrachloride as solvent, m (methyl salicylate): m (mass fraction of 65% nitric acid): m (catalyst) = 3.04: - methyl nitrosalicylate yield of 81.5%, methyl 3-nitrosalicylate yield of 12.4%, the total yield of 93.9%; catalyst recovery is easy, and after repeated use of 5 times, the activity is essentially the same .