The Kizhner Research Center, National Research Tomsk Polytechnic University, 30 Lenin Avenue, Tomsk, 634050, Russia.
Chemistry and Biochemistry Department, Montana State University, Bozeman, 59717, USA.
J Mol Model. 2021 Sep 29;27(10):305. doi: 10.1007/s00894-021-04914-x.
Although acid-catalyzed intramolecular rearrangement of organic azides is an attractive route to amines, its mechanism and synthetic prospective are still debated. Herein, through computational and experimental studies, we demonstrated that azide intramolecular rearrangement could serve as a potent synthetic route to a sought-after amine functionality including preparation of difficult to access and valuable heterocyclic amines. Using quantum chemical calculations at MP2/aug-cc-pVTZ and B3LYP/aug-cc-pVDZ levels, we discovered that this reaction proceeds via a concerted transition state with nitrogen elimination and alkyl/aryl migration occurring at the same time. Two conformers of protonated azides - syn- and anti- - were shown to precede corresponding transition states. It was shown that the reaction follows Curtin-Hammett scenario as the energy gap required for conformer interconversion was substantially lower than activation barrier of either transition state. Intramolecular amination via azide rearrangement was predicted to be a selective process with migratory aptitude increasing in a row alkyl<Ar-EWG<Ar-EDG (EWG - electron withdrawing group; EDG - electron donating group), which was supported by experimental results. We demonstrated experimentally that organic azides can be generated from stilbenes in situ and selectively undergo rearrangement to corresponding amines in a cascade fashion via amino-dealkenylation reaction.
尽管酸催化的有机叠氮化物的分子内重排是胺的一种有吸引力的合成途径,但它的机制和合成前景仍存在争议。在此,通过计算和实验研究,我们证明了叠氮化物的分子内重排可以作为一种有效的合成途径,用于合成包括难以获得和有价值的杂环胺在内的所需胺基官能团。通过在 MP2/aug-cc-pVTZ 和 B3LYP/aug-cc-pVDZ 水平上的量子化学计算,我们发现该反应通过氮消除和烷基/芳基迁移同时发生的协同过渡态进行。质子化叠氮化物的两种构象 - 顺式和反式 - 被证明先于相应的过渡态。结果表明,该反应遵循 Curtin-Hammett 情景,因为构象转化所需的能量间隙远低于任何过渡态的活化能垒。通过叠氮化物重排进行的分子内胺化被预测是一种选择性过程,迁移能力依次增加,烷基<Ar-EWG<Ar-EDG(EWG - 吸电子基团;EDG - 供电子基团),这得到了实验结果的支持。我们通过实验证明,有机叠氮化物可以从芪原位生成,并通过氨基脱烯丙基化反应以级联方式选择性地重排成相应的胺。