Hosoya Takashi, Takano Toshiyuki, Kosma Paul, Rosenau Thomas
Department of Chemistry, University of Natural Resources and Life Sciences , Muthgasse 18, A-1190 Vienna, Austria.
J Org Chem. 2014 Sep 5;79(17):7889-94. doi: 10.1021/jo501012s. Epub 2014 Aug 18.
Glycoside formation in organic synthesis is believed to occur along a reaction path involving an activated glycosyl donor with a covalent bond between the glycosyl moiety and the leaving group, followed by formation of contact ion pairs with the glycosyl moiety loosely bound to the leaving group, and eventually solvent-separated ion pairs with the glycosyl moiety and the leaving group being separated by solvent molecules. However, these ion pairs have never been experimentally observed. This study investigates the formation of the ion pairs from a covalent intermediate, 2,3,4,6-tetra-O-methyl-α-d-glucopyranosyl triflate, by means of computational chemistry. Geometry optimization of the ion pairs without solvent molecules resulted in re-formation of the covalent α- and β-triflates but was successful when four solvent (dichloromethane) molecules were taken into account. The DFT(M06-2X) computations indicated interconversion between the α- and β-covalent intermediates via the α- and β-contact ion pairs and the solvent-separated ion pairs. The calculated activation Gibbs energy of this interconversion was quite small (10.4-13.5 kcal/mol). Conformational analyses of the ion pairs indicated that the oxacarbenium ion adopts (4)H3, (2)H3/E3, (2)H3/(2)S0, E3, (2,5)B, and B2,5 pyranosyl ring conformations, with the stability of the conformers being strongly dependent on the relative location of the counteranion.
有机合成中的糖苷形成被认为是沿着一条反应路径发生的,该路径涉及一个活化的糖基供体,其糖基部分与离去基团之间存在共价键,随后形成接触离子对,其中糖基部分与离去基团松散结合,最终形成溶剂分隔离子对,糖基部分和离去基团被溶剂分子隔开。然而,这些离子对从未被实验观察到。本研究通过计算化学方法研究了由共价中间体2,3,4,6-四-O-甲基-α-D-吡喃葡萄糖基三氟甲磺酸酯形成离子对的过程。在不考虑溶剂分子的情况下对离子对进行几何优化,结果导致共价α-和β-三氟甲磺酸酯重新形成,但当考虑四个溶剂(二氯甲烷)分子时则成功了。DFT(M06-2X)计算表明,α-和β-共价中间体通过α-和β-接触离子对以及溶剂分隔离子对相互转化。计算得到的这种相互转化的活化吉布斯自由能相当小(10.4 - 13.5千卡/摩尔)。对离子对的构象分析表明,氧碳鎓离子采取(4)H3、(2)H3/E3、(2)H3/(2)S0、E3、(2,5)B和B2,5吡喃糖环构象,构象异构体的稳定性强烈依赖于抗衡离子的相对位置。