{"title":"HFIP 介导的肟醚合成:一种不含金属、碱和添加剂的方法。","authors":"Dibyashree Dolakasharia, Utpal Bora","doi":"10.1039/d4ob01556h","DOIUrl":null,"url":null,"abstract":"<p><p>Oxime ethers are extensively present as key components in numerous active pharmaceutical ingredients and many other synthetically viable organic compounds. Herein, we present a metal, base and additive free mild C-O bond formation strategy for the synthesis of oxime ethers from various oxime derivatives and tertiary and secondary aryl alcohols. The reaction is carried out in the presence of 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) as the green solvent at 30 °C. The reaction tolerates both aldoximes and ketoximes including ketoximes bearing heteroatoms, furnishing high yields (up to 99%). The formation of a triphenylmethyl carbocation as an intermediate is supported <i>via</i> UV-Vis spectroscopy. Successful gram-scale synthesis of the oxime ether, low energy input and simple reaction conditions further highlight the potential of this reaction to effectively transition from the laboratory scale to industrial production. A broad substrate scope compatibility was also observed.</p>","PeriodicalId":96,"journal":{"name":"Organic & Biomolecular Chemistry","volume":" ","pages":""},"PeriodicalIF":2.9000,"publicationDate":"2024-11-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"HFIP mediated oxime ether synthesis: a metal, base and additive free approach.\",\"authors\":\"Dibyashree Dolakasharia, Utpal Bora\",\"doi\":\"10.1039/d4ob01556h\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>Oxime ethers are extensively present as key components in numerous active pharmaceutical ingredients and many other synthetically viable organic compounds. Herein, we present a metal, base and additive free mild C-O bond formation strategy for the synthesis of oxime ethers from various oxime derivatives and tertiary and secondary aryl alcohols. The reaction is carried out in the presence of 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) as the green solvent at 30 °C. The reaction tolerates both aldoximes and ketoximes including ketoximes bearing heteroatoms, furnishing high yields (up to 99%). The formation of a triphenylmethyl carbocation as an intermediate is supported <i>via</i> UV-Vis spectroscopy. Successful gram-scale synthesis of the oxime ether, low energy input and simple reaction conditions further highlight the potential of this reaction to effectively transition from the laboratory scale to industrial production. A broad substrate scope compatibility was also observed.</p>\",\"PeriodicalId\":96,\"journal\":{\"name\":\"Organic & Biomolecular Chemistry\",\"volume\":\" \",\"pages\":\"\"},\"PeriodicalIF\":2.9000,\"publicationDate\":\"2024-11-21\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Organic & Biomolecular Chemistry\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://doi.org/10.1039/d4ob01556h\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, ORGANIC\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Organic & Biomolecular Chemistry","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1039/d4ob01556h","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, ORGANIC","Score":null,"Total":0}
引用次数: 0
摘要
肟醚作为关键成分广泛存在于多种活性药物成分和许多其他可合成的有机化合物中。在此,我们提出了一种无金属、无碱、无添加剂的温和 C-O 键形成策略,用于从各种肟衍生物和三级及二级芳基醇合成肟醚。反应是在 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) 作为绿色溶剂的情况下于 30 °C 进行的。该反应既可生成醛肟,也可生成酮肟,包括含有杂原子的酮肟,产率高(达 99%)。紫外可见光谱支持了三苯甲基羰基化合物作为中间体的形成。成功合成肟醚的克级规模、低能量输入和简单的反应条件进一步凸显了该反应从实验室规模有效过渡到工业生产的潜力。此外,该反应还具有广泛的底物兼容性。
HFIP mediated oxime ether synthesis: a metal, base and additive free approach.
Oxime ethers are extensively present as key components in numerous active pharmaceutical ingredients and many other synthetically viable organic compounds. Herein, we present a metal, base and additive free mild C-O bond formation strategy for the synthesis of oxime ethers from various oxime derivatives and tertiary and secondary aryl alcohols. The reaction is carried out in the presence of 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) as the green solvent at 30 °C. The reaction tolerates both aldoximes and ketoximes including ketoximes bearing heteroatoms, furnishing high yields (up to 99%). The formation of a triphenylmethyl carbocation as an intermediate is supported via UV-Vis spectroscopy. Successful gram-scale synthesis of the oxime ether, low energy input and simple reaction conditions further highlight the potential of this reaction to effectively transition from the laboratory scale to industrial production. A broad substrate scope compatibility was also observed.