间苯三酚的合成及表征

以三硝基甲苯(TNT)为原料,经过氧化、催化氢化、水解等步骤合成间苯三酚。并通过红外、核磁对它的结构进行了确证。考察了氧化剂以及用量、催化剂用量、溶剂、反应温度等对合成间苯三酚的影响。较佳工艺条件:HNO3-KC lO3为氧化剂,氧化剂用量与TNT用量比为2∶1。水-丙酮为催化氢化溶剂,催化剂用量约为反应物的8%,控制温度在60℃,反应2.5 h。水解pH=3~4,反应16~20 h。总收率达到60%,纯度达到98%。

Synthesis and characterization of phloroglucinol

Using trinitrotoluene as base material,phloroglucinol was synthesized through oxidation,catalytic hydrogenation,hydrolyzing.Its structure was analysized and authenticed by IR,1H NMR and 13C NMR.The effects of oxidant,dosage of oxidant and catalyst,solvent,reaction temperature on the synthesis were studied.The better technology has been obtained as follows:taking nitric acid-chlorate liquor as oxidant,ratio of dosage of it to trinitrotoluene is 2 ∶1.Taking water-acetone as solvent,the amount of catalyst is 8% of the material,reaction temperature is 60 ℃,reaction time is 2.5 h on the catalytic hydrogenation reaction.At hydrolytic reaction pH is 3~4,reaction time is 16~20 h.The yield of phloroglucinol could reach 60%.The purity of phloroglucinol is 98%.