2,6-二叔丁基-4-亚硝基苯酚的合成及表征

Synthesis and characterization of 2,6-di-tert-butyl-4-nitrosophenol

以2,6-二叔丁基苯酚、浓硫酸及亚硝酸钠为原料,在乙醇中合成了抗氧剂中间体2,6-二叔丁基-4-亚硝基苯酚,考察了溶剂种类、反应温度、反应时间、投料比和投料次序对反应的影响。结果表明,最佳工艺条件为:乙醇为溶剂,反应温度25℃,n(2,6-二叔丁基苯酚)∶n(浓硫酸)∶n(亚硝酸钠)=1∶1.1∶1.1,投料次序为先滴加浓硫酸,再滴加亚硝酸钠溶液,反应时间为2 h。在该条件下,产物重结晶收率为92.0%,产物色谱纯度≥99.7%。

The antioxidant intermediate compound 2,6-di-tert-butyl-4-nitrosophenol was synthesized, the reaction of 2,6-di-tert-butylphenol with concentration sulfuric acid and sodium nitrite as raw materials. The effects of the type of solvent, reaction temperature, reaction time, mole ratio of materials, and feeding sequence was investigated respectively. The results showed that the optimum process conditions with the yield of 92.0% and purity of 99.7 % ： ethanol as solvent, reaction temperature 25 ℃, n （ 2,6-di-tert-butyl- phenol） ： n（ concentration sulfuric acid）： n（sodium nitrite） = 1： 1. 1：1.1, the reaction system of concen- tration sulfuric acid and phenol was added dropwise of the solution of sodium nitrite,reaction time 2 h.