摘要
以邻硝基苯胺为原料,经乙酰化、甲基化、水解三步反应合成得到了目标产物2-甲基-6-硝基苯胺,并采用IR,1 H NMR和13 C NMR对产物结构进行了表征.探讨了乙酰化反应时催化剂AlCl3用量、反应温度及反应时间和滴加乙酸酐速率对邻硝基乙酰苯胺产率的影响,以及甲基化反应中催化剂AlCl3用量、反应温度、反应时间和滴加硫酸二甲酯速率对产物产率的影响.在最佳合成条件下,2-甲基-6-硝基苯胺的产率可达93.9%.
With o- nitroaniline as raw material, through acetylation, methylation, hydrolysis reactions, the target com- pound 2 - methyl - 6 - nitroaniline was synthesized and characterized by IR, 1_H NMR and 13_C NMR. In the acetylation reac- tion, the influence of dosage of catalyst A1C13, reaction temperature,reaction time and adding rate of acetic anhydride on the yield of intermediate O - nitroacetanilide was investigated. In the methylation reaction, the influence of dosage of catalyst AIC13, reaction temperature, reaction time and adding rate of dimethyl sulfate on the yield of 2 -methyl -6 -nitroaniline were investigated. Under the optimal conditions, the yield of 2 -methyl- 6 -nitroaniline was 93.9%.
出处
《周口师范学院学报》
CAS
2013年第5期71-75,共5页
Journal of Zhoukou Normal University
