<p>Duloxetine, a prominent&#xa0;5-hydroxytryptamine norepinephrine reuptake inhibitor, is deployed mainly in the management of adult depression, showcasing minimal side effects, swift therapeutic onset, and a robust safety profile. Ethyl (<i>S</i>)-3-hydroxy-3-(2-thienyl)propionate ((<i>S</i>)-HEES) is the crucial chiral intermediate for duloxetine production. Asymmetric synthesis of (<i>S</i>)-HEES using carbonyl reductase as the biocatalyst has exhibited advantages including mild reaction conditions, high catalytic efficiency and environmental friendliness. In the present study, a loop region alteration strategy was developed to screen for a carbonyl reductase for (<i>S</i>)-HEES synthesis and <i>Ea</i>SDR6 from <i>Exiguobacterium</i> sp. s126 was identified with considerable catalytic performance and broad substrate adaptability. Site-directed mutagenesis&#xa0;was subsequently performed, Mut-R142A/N204A was identified with a 3.6-fold enhancement in activity relative to the wild-type <i>Ea</i>SDR6. The mutant <i>k</i><sub>cat</sub> value was 52.5&#xa0;s<sup>−1</sup>, 2.9-fold compared to the wild type, and the total catalytic efficiency (<i>k</i><sub>cat</sub>/<i>K</i><sub>M</sub>) was 24.9&#xa0;mM<sup>−1</sup>&#xa0;s<sup>−1</sup>, 1.9-fold higher than the wild type. The <i>n</i>-butyl acetate–aqueous biphasic bioreaction system was established for the asymmetric synthesis of (<i>S</i>)-HEES with the conversion of ethyl 3-oxo-3-(2-thienyl)propionate (KEES) of 90.2%, the product e.e. of &gt; 99% after 8&#xa0;h reaction at a substrate concentration of 200&#xa0;g/L. The spatiotemporal yield reached 22.5&#xa0;g/(L·h), which was higher than the ever reports about (<i>S</i>)-HEES biosynthesis. The present research provides new knowledge and technology for the construction of stereoselective carbonyl reductase and the green biosynthesis of chiral alcohol pharmaceutical intermediates.</p> Graphical abstract <p></p>

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Modification of carbonyl reductase based on substrate pocket loop regions alteration: an application for synthesis of duloxetine chiral intermediate in high efficiency

  • Xiao-Jian Zhang,
  • Kai-Li Chen,
  • Xiang-Yang Li,
  • Qi-Qi Yuan,
  • Chao-Ping Lin,
  • Zhi-Qiang Liu,
  • Yu-Guo Zheng

摘要

Duloxetine, a prominent 5-hydroxytryptamine norepinephrine reuptake inhibitor, is deployed mainly in the management of adult depression, showcasing minimal side effects, swift therapeutic onset, and a robust safety profile. Ethyl (S)-3-hydroxy-3-(2-thienyl)propionate ((S)-HEES) is the crucial chiral intermediate for duloxetine production. Asymmetric synthesis of (S)-HEES using carbonyl reductase as the biocatalyst has exhibited advantages including mild reaction conditions, high catalytic efficiency and environmental friendliness. In the present study, a loop region alteration strategy was developed to screen for a carbonyl reductase for (S)-HEES synthesis and EaSDR6 from Exiguobacterium sp. s126 was identified with considerable catalytic performance and broad substrate adaptability. Site-directed mutagenesis was subsequently performed, Mut-R142A/N204A was identified with a 3.6-fold enhancement in activity relative to the wild-type EaSDR6. The mutant kcat value was 52.5 s−1, 2.9-fold compared to the wild type, and the total catalytic efficiency (kcat/KM) was 24.9 mM−1 s−1, 1.9-fold higher than the wild type. The n-butyl acetate–aqueous biphasic bioreaction system was established for the asymmetric synthesis of (S)-HEES with the conversion of ethyl 3-oxo-3-(2-thienyl)propionate (KEES) of 90.2%, the product e.e. of > 99% after 8 h reaction at a substrate concentration of 200 g/L. The spatiotemporal yield reached 22.5 g/(L·h), which was higher than the ever reports about (S)-HEES biosynthesis. The present research provides new knowledge and technology for the construction of stereoselective carbonyl reductase and the green biosynthesis of chiral alcohol pharmaceutical intermediates.

Graphical abstract