Lanza Lucrezia, Bjarnesen Daniela, Çakar Mehmet Mervan, Rizzo Andrea, Pandya Akash, Aranda Carmen, Blažević Zvjezdana Findrik, Müller Michael
Institute of Pharmaceutical Sciences, Albert-Ludwigs-Universität Freiburg, Albertstrasse 25, Freiburg, 79104, Germany.
Faculty of Chemical Engineering and Technology, University of Zagreb, Trg Marka Marulića 19, Zagreb, 10000, Croatia.
Chemistry. 2025 Jun 23;31(35):e202500890. doi: 10.1002/chem.202500890. Epub 2025 Jun 8.
The development of (bio)catalytic methods to chiral tertiary alcohols is in demand, yet the enantioselective synthesis of tertiary alcohols with sterically hindered moieties is problematic. JanthE is a novel thiamine diphosphate-dependent enzyme that catalyzes aldehyde-ketone cross-coupling reactions with a wide range of donor and acceptor substrates. However, product formation is low and precludes large-scale production. We investigated the conversion of 2-oxobutanoate and the bulky ketone phenoxy-2-propanone to the product 2-hydroxy-2-methyl-1-phenoxypentan-3-one as a model reaction for the synthetic capabilities of JanthE. As the reaction design did not significantly improve the yield, we proceeded to rational protein engineering. Docking experiments identified V121, Y268, P293, Y297, and K567 in the active site as important residues for catalysis. Remarkably, the single-point variant JanthE K567S led to a fivefold increase in product formation (90% ee) compared to the wild type enzyme (93% ee). The reaction was performed at preparative scale proving the direct possibility of application. Additionally, when the reaction was extended to longer 2-oxopentanoate, the double variant Y297P_K567S showed a 5-fold increase in product formation compared to the wild type. Our results demonstrate the evolvability and versatility of JanthE for the enantioselective synthesis of sterically hindered tertiary alcohols.
开发用于合成手性叔醇的(生物)催化方法很有必要,然而,对带有空间位阻基团的叔醇进行对映选择性合成存在问题。JanthE是一种新型的依赖硫胺二磷酸的酶,可催化醛 - 酮交叉偶联反应,底物范围广泛,包括供体和受体。然而,产物生成量较低,阻碍了大规模生产。我们研究了以2-氧代丁酸酯和位阻较大的酮苯氧基-2-丙酮转化为产物2-羟基-2-甲基-1-苯氧基戊-3-酮作为JanthE合成能力的模型反应。由于反应设计未能显著提高产率,我们进而进行了合理的蛋白质工程改造。对接实验确定活性位点中的V121、Y268、P293、Y297和K567是催化的重要残基。值得注意的是,单点变体JanthE K567S与野生型酶(对映体过量值为93%)相比,产物生成量增加了五倍(对映体过量值为90%)。该反应在制备规模上进行,证明了其直接应用的可能性。此外,当反应扩展到更长链的2-氧代戊酸酯时,双变体Y297P_K567S与野生型相比,产物生成量增加了5倍。我们的结果证明了JanthE在对映选择性合成空间位阻叔醇方面的可进化性和多功能性。