第 38 卷第 4 期 | | Vol. 38 No. 4 | 2008 年 8 月 | Aug 2008 |
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所属栏目:农药及中间体
高效除草剂双草醚中间体2,6-双(4,6-二甲氧嘧啶氧基)苯甲酸的合成 |
李元祥1,2
(1. 湖南怀化学院 化学化工系,湖南 怀化 418008;2. 华中师范大学 化学学院农药与化学生物学教育部重点实验室,湖北 武汉 430079) |
摘 要:以2,6-二羟基苯甲酸为原料,与无水甲醇在浓硫酸或三氟化硼-乙醚的催化下制备2,6-二羟基苯甲酸甲酯,收率分别为43.5%、46%;2,6-二羟基苯甲酸甲酯再与4,6-二甲氧基-2-甲磺酰嘧啶(DMSP)在碳酸钾丙酮条件下反应生成2,6-双(4,6-二甲氧嘧啶氧基)苯甲酸甲酯,收率91.5%;所得中间体经20%的氢氧化钾水溶液水解后由0.7%的柠檬酸酸化后生成2,6-双(4,6-二甲氧嘧啶氧基)苯甲酸,收率72%。 |
关键词:除草剂;双草醚;中间体;合成 |
中图分类号:TQ457.29 文献标识码:A 文章编号:1009-9212(2008)04- 0021-04 |
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Synthesis of Intermediate 2,6-Bis(4,6-dimethoxypyrimidin-2-yloxy)benzoate for Herbicide Bispyribac-sodium |
LI Yuan-xiang1,2
(1. Chemistry and Chemical Engineering Department,Huaihua University,Huaihua 418008,China;2. Key Laboratory of Pesticide & Chemical Biology,Ministry of Education,College of Chemistry,Central China Normal University,Wuhan 430079,China) |
Abstract:Methyl 2,6-dihydroxybenzoate was first synthesized with 2,6-dihydroxybenzoic acid as the raw materials through reaction of absolute methanol in the presence of the strong sulfuric acid or BF3·Et2O,the yield was 43.5% and 46% respectively. Then methyl 2,6-bis(4,6-dimethoxy-pyrimidin-2-yloxy)benzoate was synthesized from methyl 2,6-dihydroxy-benzoate and 4,6-dimethoxy-2-(methylsulfonyl)pyrimidine(DMSP) in the presence of K2CO3 in acetone,and the yield was 91.5%. The previous intermediate can be formed 2,6-bis(4,6-dimeth-oxypyrimidin-2-yloxy)benzoic acid via hydrolyzation with the 20% KOH and acidification with the 0.7 % citric acid,and the yield was 72%. |
Key words:herbicide;bispyribac-sodium;intermediates;synthesis |
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作者简介:李元祥(1968-),男,湖南怀化人,讲师,博士,主要从事新型农药分子的设计与合成。(E-mail:liyuanjun68@yahoo.com.cn)
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收稿日期:2008-08-04
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