CAJ | 학술논문

环己氧基-4-氧-2,2,6,6-四甲基哌啶酮是合成具有优异阻燃性能的受阻胺类阻燃剂的关键中间体.研究在前人工作的基础上,探索新的工艺合成路线.先按已有的方法合成2,2,6,6-四甲基哌啶氮氧自由基,再以环己烷和2,2,6,6-四甲基哌啶氮氧自由基为原料,叔丁基过氧化氢和溴化铜为氧化-还原引发体系,四丁基溴化铵为相转移催化剂合成了1-环己氧基-4-氧-2,2,6,6-四甲基哌啶酮.用电子自旋共振谱仪(ESR)和电喷雾质谱仪(ESI-MS)对产物进行了相应表征.实验研究了反应工艺、金属催化剂和相转移催化剂对产率的影响,并对反应机理进行了探讨.研究结果表明,该合成方法的产率可达到82%.
배기양기-4-양-2,2,6,6-사갑기고정동시합성구유우이조연성능적수조알류조연제적관건중간체.연구재전인공작적기출상,탐색신적공예합성로선.선안이유적방법합성2,2,6,6-사갑기고정담양자유기,재이배기완화2,2,6,6-사갑기고정담양자유기위원료,숙정기과양화경화추화동위양화-환원인발체계,사정기추화안위상전이최화제합성료1-배기양기-4-양-2,2,6,6-사갑기고정동.용전자자선공진보의(ESR)화전분무질보의(ESI-MS)대산물진행료상응표정.실험연구료반응공예、금속최화제화상전이최화제대산솔적영향,병대반응궤리진행료탐토.연구결과표명,해합성방법적산솔가체도82%.
Sterically hindered amine shows great advantages among the various kinds of flame retardants.1-cyclohexyloxy-2,2,6,6- tetramethylpipirid-4-one is the key intermediate for synthesizing this kind of flame retardant. In this paper, we proposed a novel method for synthesizing 1-cyclohexyloxy-2,2,6,6-tetramethylpipirid-4-one with a higher yield. First, sterically hindered nitroxyl radical was synthesized by using the existing method. Then, cyclohexane and the obtained nitroxyl radical were used to synthesize 1-cyclohexyloxy-2,2,6,6- tetramethylpipirid-4-one. Tert-butyl hydroperoxide and copper bromide were employed as the redox initiator system and tetrabutyl ammonium bromide as the phase transfer catalyst. The target product was characterized by electron-spin resonance(ESR) and electro spray ionization-mass spectroscopy(ESI-MS). The effects of metal catalyst and phase transfer catalyst on product yield were investigated. The catalytic mechanism of the reaction was also studied. The product yield using this method can reach 82%.