Fossey-Jouenne Aurélie, Vergne-Vaxelaire Carine, Zaparucha Anne
Génomique Métabolique, Genoscope, Institut François Jacob, CEA, CNRS, Univ Evry, Univ Paris-Saclay.
Génomique Métabolique, Genoscope, Institut François Jacob, CEA, CNRS, Univ Evry, Univ Paris-Saclay;
J Vis Exp. 2018 Feb 16(132):56926. doi: 10.3791/56926.
Amino alcohols are versatile compounds with a wide range of applications. For instance, they have been used as chiral scaffolds in organic synthesis. Their synthesis by conventional organic chemistry often requires tedious multi-step synthesis processes, with difficult control of the stereochemical outcome. We present a protocol to enzymatically synthetize amino alcohols starting from the readily available L-lysine in 48 h. This protocol combines two chemical reactions that are very difficult to conduct by conventional organic synthesis. In the first step, the regio- and diastereoselective oxidation of an unactivated C-H bond of the lysine side-chain is catalyzed by a dioxygenase; a second regio- and diastereoselective oxidation catalyzed by a regiodivergent dioxygenase can lead to the formation of the 1,2-diols. In the last step, the carboxylic group of the alpha amino acid is cleaved by a pyridoxal-phosphate (PLP) decarboxylase (DC). This decarboxylative step only affects the alpha carbon of the amino acid, retaining the hydroxy-substituted stereogenic center in a beta/gamma position. The resulting amino alcohols are therefore optically enriched. The protocol was successfully applied to the semipreparative-scale synthesis of four amino alcohols. Monitoring of the reactions was conducted by high performance liquid chromatography (HPLC) after derivatization by 1-fluoro-2,4-dinitrobenzene. Straightforward purification by solid-phase extraction (SPE) afforded the amino alcohols with excellent yields (93% to >95%).
氨基醇是用途广泛的化合物,具有多种应用。例如,它们已被用作有机合成中的手性支架。通过传统有机化学合成它们通常需要繁琐的多步合成过程,且立体化学结果难以控制。我们提出了一种在48小时内从易于获得的L-赖氨酸酶促合成氨基醇的方案。该方案结合了两个传统有机合成很难进行的化学反应。第一步,赖氨酸侧链未活化的C-H键的区域和非对映选择性氧化由双加氧酶催化;由区域发散双加氧酶催化的第二步区域和非对映选择性氧化可导致1,2-二醇的形成。在最后一步,α-氨基酸的羧基由磷酸吡哆醛(PLP)脱羧酶(DC)裂解。该脱羧步骤仅影响氨基酸的α-碳,将羟基取代的立体中心保留在β/γ位置。因此,所得的氨基醇具有光学富集性。该方案已成功应用于四种氨基醇的半制备规模合成。反应监测通过1-氟-2,4-二硝基苯衍生化后的高效液相色谱(HPLC)进行。通过固相萃取(SPE)直接纯化得到的氨基醇产率极高(93%至>95%)。