| 2,2-二氟苯并[1,3]间二氧杂环戊烯-4-甲醛的合成 |
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| 引用本文： | 刘少春,廖道华,杜梦,吴贯中,刘丙祥,张曙光,陈倩.2,2-二氟苯并[1,3]间二氧杂环戊烯-4-甲醛的合成[J].农药,2011,50(5). |
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| 作者姓名： | 刘少春 廖道华 杜梦 吴贯中 刘丙祥 张曙光 陈倩 |
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| 作者单位： | 华东理工大学药学院,上海,200237 |
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| 摘 要： | 目的]旨在优化出一条适合工业化生产2,2-二氟苯并1,3]问二氧杂环戊烯-4-甲醛的工艺路线.方法]以邻甲酚为起始原料.经"一锅煮"得到3-甲基苯邻二酚,再经醚化、氯化、氟交换和水解5步反应得2,2-二氟苯并1,3]间二氧杂环戊烯-4-甲醛.结果]反应总收率35.1%,含量99.5%(GC),产物与中间体经1H NMR、MS等进行了表征.结论]提高了收率,简化了操作,适合工业化生产.
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| 关 键 词： | 2 2-二氟苯并[1 3]间二氧杂环戊烯-4-甲醛 咯菌腈 杀菌剂 合成 |
Synthesis of 2,2-Difluoro-1,3-benzodioxol-4-aldehyde |
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| LIU Shao-chun,LIAO Dao-hua,DU Meng,WU Guan-zhong,LIU Bing-xiang,ZHANG Shu-guang,CHEN Qian.Synthesis of 2,2-Difluoro-1,3-benzodioxol-4-aldehyde[J].Pesticides,2011,50(5). |
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| Authors: | LIU Shao-chun LIAO Dao-hua DU Meng WU Guan-zhong LIU Bing-xiang ZHANG Shu-guang CHEN Qian |
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| Affiliation: | LIU Shao-chun,LIAO Dao-hua,DU Meng,WU Guan-zhong,LIU Bing-xiang,ZHANG Shu-guang,CHEN Qian(Pharmacy School,East China University of Science and Technology,Shanghai 200237,China) |
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| Abstract: | This article aims to optimize a reasonable route of 2,2-difluoro-1,3-benzodioxol-4-aldehyde onindustrial scale.Methods]2,2-Difluoro-1,3-benzodioxol-4-aldehyde was synthesized from o-cresol as starting materialvia five steps including one pot synthesis of 3-methyl-1,2-benzene-diol,and then etherification,chlorination,fluorination,and hydrolysis.Results]The total yield was 35.1%,and the purity of the target product was up to 99.5%(GC).Theproducts and intermediates were determined by1H NMR and MS and so on.... |
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| Keywords: | 2 2-difluoro-1 3-benzodioxol-4-aldehyde fludioxonil fungicide synthesis |
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