丁基吡啶四氟硼酸盐中的两相Beckmann重排反应

在丁基吡啶四氟硼酸盐([bupy][BF4])/甲苯两相体系中,以含磷化合物(PICl3,PCl3,PCl5)催化环己酮肟的Beckmann重排反应。考察了催化剂和离子液体用量、物料配比、反应时间、反应温度等条件对环己酮肟转化率、己内酰胺选择性的影响。结果表明,POCl3催化的两相重排反应结果很好,环己酮肟的转化率高达100.0％,己内酰胺的选择性高达99.3％。并优化出POCl3催化的两相重排反应条件。在两相体系中进行重排反应有利于控制反应速率和实现体系取热。

Beckmann Rearrangement of Cyclohexanone Oxime in Two-Phase System Consisted of n -Butyl-Pyridinium Tetrafluoroborate and Toluene

Beckmann rearrangement of cyclohexanone oxime in the two-phase system consisted of n -butyl-pyridinium tetrafluoroborate ([bupy] [BF4]) and toluene using phosphorous compounds (POCl3, PCl3, PCl5) as catalyst were studied. Effects of amount of cyclohexanone oxime, catalyst and ionic liquids, ratios between above materials, reaction time and reaction temperature on conversion of cyclohexanone oxime and selectivity of ε -caprolactam were investigated. Conversion of cyclohexanone oxime could reach 100.0% , while selectivity of ε-caprolactam could reach 99.3% , which showed that the result of two-phase rearrangement catalyzed by POC13 was excellent. Reaction conditions catalyzed by POC13 were optimized. The above two -phase system facilitated control of reaction rate and removal of reaction heat.