Córdova Armando, Sundén Henrik, Bøgevig Anders, Johansson Mikael, Himo Fahmi
Department of Organic Chemistry, The Arrhenius Laboratory, Stockholm University, 106 91 Stockholm, Sweden.
Chemistry. 2004 Aug 6;10(15):3673-84. doi: 10.1002/chem.200400137.
Proline-catalyzed direct asymmetric alpha-aminooxylation of ketones and aldehydes is described. The proline-catalyzed reactions between unmodified ketones or aldehydes and nitrosobenzene proceeded with excellent diastereo- and enantioselectivities. In all cases tested, the corresponding products were isolated with >95 % ees. Methyl alkyl ketones were regiospecifically oxidized at the methylene carbon atom to afford enantiomerically pure alpha-aminooxylated ketones. In addition, cyclic ketones could be alpha,alpha'-dioxidized with remarkably high selectivity, furnishing the corresponding diaminooxylated ketones with >99 % ees. The reaction mechanism of the proline-catalyzed direct asymmetric alpha-aminooxylation was investigated, and we performed density functional theory (DFT) calculations in order to investigate the nature of the plausible transition states further. We also screened other organocatalysts for the asymmetric alpha-oxidation reaction and found that several proline derivatives were also able to catalyze the transformation with excellent enantioselectivities. Moreover, stereoselective routes for the synthesis of monoprotected vicinal diols and hydroxyketones were found. In addition, short routes for the direct preparation of enantiomerically pure epoxides and 1,2-amino alcohols are presented. The direct catalytic alpha-oxidation is also a novel route for the stereoselective preparation of beta-adrenoreceptor antagonists.
本文描述了脯氨酸催化的酮和醛的直接不对称α-氨基氧化反应。未修饰的酮或醛与亚硝基苯之间的脯氨酸催化反应具有优异的非对映选择性和对映选择性。在所有测试的情况下,相应产物的对映体过量(ee)值均大于95%。甲基烷基酮在亚甲基碳原子上进行区域特异性氧化,得到对映体纯的α-氨基氧化酮。此外,环酮可以以非常高的选择性进行α,α'-二氧化,得到对映体过量值大于99%的相应二氨基氧化酮。研究了脯氨酸催化的直接不对称α-氨基氧化反应的机理,并且我们进行了密度泛函理论(DFT)计算,以便进一步研究可能的过渡态的性质。我们还筛选了用于不对称α-氧化反应的其他有机催化剂,发现几种脯氨酸衍生物也能够以优异的对映选择性催化该转化反应。此外,还发现了合成单保护邻二醇和羟基酮的立体选择性路线。另外,还提出了直接制备对映体纯环氧化物和1,2-氨基醇的简短路线。直接催化α-氧化也是立体选择性制备β-肾上腺素能受体拮抗剂的一条新途径。