2,4,6-三氯硝基苯的合成与产物的分离纯化研究

Studies on Synthesis and the Product Isolation and Purification of 2,4,6-trichloronitrobenzene

以1,3,5-三氯苯为原料,在浓硫酸与浓硝酸的作用下硝化成2,4,6-三氯硝基苯。考察了原料配比、反应温度和反应时间,确定了最佳反应条件,在此条件下反应产物的纯度达到99%以上,反应产率达到85%以上。同时,在上述基础上进行硝基三氯苯的破坏性试验,并对可能生成的混硝基三氯苯进行薄层色谱(TCL)分离,再纯化,最后用质谱仪、红外分光光度计、核磁共振波谱仪等进行结构表征。

Technology of synthesis of 2,4,8 - trichloronitrobenzene by 1,3,5 - trichlorobenzene, sulphuric acid and nitric acid was studied. The effect of the reaction temperature, reaction time and raw material mix on the synthesis of 2,4, 6 - trichloronitrobenzene were studided, which got the suitable processing condition, the concentrations was 99 % and the yield of the reaction was 85 %. Besides the experiments were done on above - mentioned foundations, using more nitric acid which obtained mix- nitrotrichlorobenzene. Then it was isolated by TLC which employ the different polar. At last it was identified with CC, NS, IR and NMR.