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以4,6-二硝基-1,2,3-三氯苯为原料,采用水相碱性水解法合成了2-氯-4,6-二硝基间苯二酚,并采用了元素分析,红外光谱,质谱和高效液相色谱对合成的产品进行了表征。采用正交实验法对合成2-氯-4,6-二硝基间苯二酚的工艺进行了研究,确定了最佳工艺条件,在此条件下得到的2-氯-4,6-二硝基间苯二酚的收率为96.37%,纯度为96.89%。对水解产品重结晶用溶剂进行了考察,确定了正丁醇为水解产品重结晶用溶剂,重结晶产品的收率为90.02%,纯化后产品的纯度为99.56%。
Using 4,6-dinitro-1,2,3-trichlorobenzene as raw material, 2-chloro-4,6-dinitroresorcin was synthesized by aqueous alkaline hydrolysis. Analysis, IR, MS and HPLC were used to characterize the synthesized products. Orthogonal experimental method for the synthesis of 2-chloro-4,6-dinitro resorcinol process was studied to determine the optimum process conditions, under these conditions obtained 2-chloro-4,6-bis The yield of nitro resorcinol was 96.37% with a purity of 96.89%. The solvent for recrystallization of hydrolyzate was investigated. It was confirmed that n-butanol was the solvent for recrystallization of hydrolyzate. The yield of recrystallized product was 90.02%. The purity of purified product was 99.56%.