论文部分内容阅读
从2,7-二磺酸钾-9-芴酮经过碱熔、脱水两步反应,合成2,7-二羟基-9-芴酮。研究了反应时间、反应物配比、pH值、纯化溶剂的配比和用量等因素对体系的影响。最佳合成工艺条件为:碱熔反应:反应物配比w(2,7-二磺酸钾-9-芴酮)∶w(NaOH)=1∶2,反应时间5min,pH=1时产物的收率为69.01%,纯度为98.85%;脱水反应:反应物配比w(4,4′-二羟基联苯-2-甲酸)∶w(ZnCl2)=1∶2,产物2,7-二羟基-9-芴酮的收率为88.50%,纯度为96.72%;采用乙醇-水体系改进工艺,产物纯度可达98.21%。
From potassium 2,7-disulfonate-9-fluorenone through alkali melting, dehydration two-step reaction, 2,7-dihydroxy-9-fluorenone. The effects of reaction time, ratio of reactants, pH value, the ratio and amount of purified solvent on the system were studied. The optimum synthesis conditions are: alkali fusion reaction: the ratio of reactants w (potassium 2,7-disulfonate -9-fluorenone): w (NaOH) = 1: 2, reaction time 5min, pH = 1 The yield was 69.01% and the purity was 98.85%. The dehydration reaction: the ratio of the reactants w (4,4’-dihydroxybiphenyl-2-carboxylic acid): w The yield of dihydroxy-9-fluorenone was 88.50% and the purity was 96.72%. The purity of the product reached 98.21% with the improvement of ethanol-water system.