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作 者:吴文陵[1] 林明穗[1] 王仁章[1] 剧丽楠[1]
机构地区:[1]三明学院化学与生物工程学院,福建三明365004
出 处:《宝鸡文理学院学报(自然科学版)》2012年第4期29-32,35,共5页Journal of Baoji University of Arts and Sciences(Natural Science Edition)
基 金:福建省科技创新平台项目(2010H2006);三明学院自然科学基金项目(B0907/Q);三明学院质量工程创新基金项目(ZL1121/CS)
摘 要:目的研究离子液体1-丁基-3-甲基咪唑六氟磷酸盐作为相转移催化剂,以五氯吡啶(PCP)为原料合成2,3,5-三氯吡啶的适宜条件。方法利用单因素实验法分析相转移催化剂、反应温度、反应时间、NaOH浓度、nZn∶nPCP等因素对产物收率的影响。结果制备2,3,5-三氯吡啶的适宜实验条件:相转移催化剂用量3mmol,反应温度40℃,反应时间5h,NaOH浓度7mol/L,nZn∶nPCP=3.0∶1。此条件下,产物收率可达75%以上。结论利用离子液体替代传统有机溶剂作为相转移催化剂合成新工艺,具有反应时间短,锌粉用量少,反应温度温和等特点,可达到绿色生产之目的。Aim To study the favorable synthesis conditions of 2, 3, 5-trichloropyridine been syn- thesized with 1-butyl-3-methylimidazolium hexafluorophosphate (BMIMPF6) as phase transfer cata- lyst using pentachloropyridine(PCP). Methods Single factor methods is used to investigate phase transfer catalyst, reaction temperature, reaction time, concentration of sodium hydroxyl , the mole ratio of zinc to pentachloropyridine on the yield of 2, 3, 5-trichloropyridine. Results Favorable syn- thesis conditions of this product are as follow: dosage of catalyst is 3 mmol, reaction temperature is 40 ℃, reaction time is 5 h, concentration of NaOH was 7 mol/L , the mole ratio of zinc to PCP is 3.0 to 1. Under the conditions, The yield of 2, 3, 5-trichloropyridine was above 75%. Conclusion The re- suits showed that reaction time was shortened and mole ratio of zinc to PCP reduced and reaction tem- perature lower with 1-butyl-3-methylimidazolium hexafluorophosphate (BMIMPF6) as phase transfer catalyst.
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