第 37 卷第 2 期 | | Vol. 37 No. 2 | 2007 年 4 月 | Apr 2007 |
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所属栏目:农药及中间体
4-氨基-3,5-二氯-2,6-二氟吡啶的合成研究 |
杨剑波,庞怀林,黄超群,陶贤鉴
(湖南化工研究院,湖南 长沙 410007) |
摘 要:以3,5-二氯-2,4,6-三氟吡啶(TFP)为原料,水为溶剂,采用带压氨解合成氟草烟的中间体4-氨基-3,5-二氯-2,6-二氟吡啶,对反应条件进行了研究,优化反应条件为:反应温度80℃,反应时间30 min,物料比n(TFP) ∶ n(氨水) = 1 ∶ 3.5,苄基三乙基氯化铵的用量为TFP质量的5%。优化反应条件下收率为83.5%,产品含量为98.6%,其结构经红外分析、元素分析、核磁共振确证。 |
关键词:3,5-二氯-2,4,6-三氟吡啶;氨化;4-氨基-3,5-二氯-2,6-二氟吡啶;合成 |
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Synthesis of 4-Amino-3,5-dichloro-2,6-difluoropyridine |
YANG Jian-bo,PANG Huai-lin,HUANG Chao-qun,Tao Xian-jian(Hunan Research Institute of Chemical Industry,Changsha 410007,China) |
Abstract:4-Amino-3,5-dichloro-2,6-difluoropyridine,an important intermediate of fluroxypyr,was synthesized from 3,5-dichloro-2,4,6-trifluoropyridine(TFP)via reaction of amination using water as the solvent and under the pressure. The optimum reaction conditions were abtained as follows. Temperature was 80℃,reaction time was 30min,the molar ratio of TFP and aqueous ammonia was 1 ∶ 3.5,the catalyst (benzyl triethyl ammonium chloride)amount was 5% comparing to TFP(m/m). The yield and purith was 83.5% and over 98.6%,respeetively. The product was confirmed by IR、elementary and 1H NMR.
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Key words:3,5-dichloro-2,4,6-trifluoropyridine;amination;4-amino-3,5-dichloro-2,6-difluoropyridine;synthesis |
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作者简介:杨剑波(1968-),女,湖南长沙人,副研究员,主要从事农药及其中间体的合成研究。(E-mail:yjb8010@sina.com)
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收稿日期:2006-12-28
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