| 2,2-二氟苯并[1,3]间二氧杂环戊烯-4-甲醛的合成新工艺 |
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| 引用本文： | 陆阳,范荣胜,陶京朝,周志莲.2,2-二氟苯并[1,3]间二氧杂环戊烯-4-甲醛的合成新工艺[J].云南化工,2011(6):45-49. |
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| 作者姓名： | 陆阳 范荣胜 陶京朝 周志莲 |
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| 作者单位： | [1]信阳农专有机化学教研室,河南信阳464000 [2]信阳市气象局,河南信阳464000 [3]郑州大学化学系,河南郑州450001 [4]河南科易集团新药研究开发中心,河南信阳464000 |
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| 摘 要： | 研究了2,2-二氟苯并1,3]间二氧杂环戊烯-4-甲醛的合成反应条件。以邻甲苯酚为原料,经"一锅煮"得到中间体3-甲基苯邻二酚,再经醚化、氯化、氟交换和水解5步反应得到2,2-二氟苯并1,3]间二氧杂环戊烯-4-甲醛,在优化的反应条件下,反应总收率为33.2%,目标产物含量99.7%,用IR、1H NMR表征了其结构。
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| 关 键 词： | 邻甲苯酚 2 2-二氟苯并[1 3]间二氧杂环戊烯-4-甲醛 氟咯菌腈 |
New Process of 2,2-Difluoro-1,3-benzodioxol-4-aldehyde |
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| Affiliation: | LU Yang,FAN Rong-sheng,TAO Jing-zhao,ZHANG Zhi-rong(1.Office of Organic chemistry,Xinyang Agriculture College,Xinyang 464000,China;2.Xinyang Atmosphere Bureau,Xinyang 464000,China;3.Chemistry Department of Zhengzhou University,Zhengzhou 450001,China;4.New Drug Research and Development Center Henan Keyi Group,Xinyang 464000,China) |
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| Abstract: | 2,2-difluoro-1,3-benzodioxol-4-aldehyde was the key intermediate of fungicide fludioxonil.The synthetic process of 2,2-difluoro-1;3-benzodioxol-4-aldehyde was studied in order to improve the yield and the purity of the product.The title compound was prepared from o-cresol as the raw material via five steps including one pot synthesis of 3-methyl-1,2-benzene-diol,and then etherification,chlorination,fluorination,and hydrolysis.Under the optimal condition,the total yield was 33.2%,and the purity was 99.7%.The structure of the resulting product was confirmed by IR、1^H NMR. |
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| Keywords: | o-cresol 2 2-difluoro-1 3-benzodioxol-4-aldehyde synthesis |
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