Berkessel Albrecht, Adrio Jens A, Hüttenhain Daniel, Neudörfl Jörg M
Institut für Organische Chemie, Universität zu Köln, Greinstrasse 4, D-50939 Köln, Germany.
J Am Chem Soc. 2006 Jul 5;128(26):8421-6. doi: 10.1021/ja0545463.
The influence of conformation and aggregation on the hydrogen bond donor ability of fluorinated alcohol solvents [1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) and 1-phenyl-2,2,2-trifluoroethanol (PhTFE)] was explored theoretically (DFT) and experimentally (NMR, kinetics, crystal structure analyses). The detailed DFT analysis revealed a pronounced dependence of the H-bond donor ability on the conformation along the CO-bond of the monomeric alcohols. The donor orbital energy (sigma*(OH)) decreases and the molecular dipole moment (mu) increases drastically from the antiperiplanar (ap) to the synperiplanar (sp) H(C)COH conformation. The kinetics of olefin epoxidation with H(2)O(2) in HFIP indicate higher order solvent aggregates (2-3 monomers) to be responsible for the activation of the oxidant. Single-crystal X-ray analyses of HFIP and PhTFE confirmed the existence of H-bonded aggregates (infinite helices, ribbons, and cyclic oligomers) and the predominance of sc to sp conformations of the fluoroalcohol monomers. These aggregate structures served as the basis for a DFT analysis of the H-bond donor ability at the terminal hydroxyl group of HFIP mono- to pentamers. Both the LUMO energy and the natural charge of the terminal hydroxyl proton indicated a substantial cooperative influence of dimerization and trimerization on the H-bond donor ability. We therefore conclude that dimers and trimers, with the individual monomers in their sc to sp conformation, play a crucial role for the solvolytic and catalytic effects exerted by HFIP, rather than monomers.
从理论(密度泛函理论,DFT)和实验(核磁共振、动力学、晶体结构分析)两方面探究了构象和聚集对含氟醇溶剂[1,1,1,3,3,3 - 六氟 - 2 - 丙醇(HFIP)和1 - 苯基 - 2,2,2 - 三氟乙醇(PhTFE)]氢键供体能力的影响。详细的DFT分析表明,氢键供体能力对单体醇沿C - O键的构象有显著依赖性。从反式共平面(ap)到顺式共平面(sp)的H(C)COH构象,供体轨道能量(σ*(OH))降低,分子偶极矩(μ)急剧增加。在HFIP中用H₂O₂进行烯烃环氧化的动力学表明,高阶溶剂聚集体(2 - 3个单体)负责氧化剂的活化。HFIP和PhTFE的单晶X射线分析证实了氢键聚集体(无限螺旋、带状和环状低聚物)的存在以及氟代醇单体sc到sp构象的优势。这些聚集结构为DFT分析HFIP单体至五聚体末端羟基的氢键供体能力提供了基础。最低未占分子轨道(LUMO)能量和末端羟基质子的自然电荷均表明二聚化和三聚化对氢键供体能力有显著的协同影响。因此,我们得出结论,由处于sc到sp构象的单个单体形成的二聚体和三聚体,而非单体,在HFIP发挥的溶剂分解和催化作用中起关键作用。