Optimization of the synthetic technology of 4,6-dinitro-1,2,3-trichlorobenzene by homogeneous design
2007
The synthesis technology of 4,6-dinitro-1,2,3trichloro-benzene was studied.Homogeneous design,which is one of the chemometric methods,was used to optimize the synthetic conditions.The results show that the reaction time is the most significant factor that can affect the yield of 4,6-dinitro-1,2,3-trichloro-benzene and then the sequence of the residual factors is as follows,the reaction temperature,the molar ratio of nitric acid to 1,2,3-trichloro-benzene,and the molar ratio of sulphuric acid to 1,2,3-trichloro-benzene.The optimized synthetic conditions are proved to be that the reaction time is 3.92 h,the reaction temperature is 62.98 ℃,the molar ratio of nitric acid to 1,2,3-trichloro-benzene is 2.31∶1 and the molar ratio of sulphuric acid to 1,2,3-trichloro-benzene is 11∶1 and the highest yield can reach to 97.95%.Furthermore the product were analyzed by HPLC,IR and elementary analysis.
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