Synthesis and Biological Evaluation of Deoxycyclophellitols as Human Retaining β-Glucosidase Inhibitors

Chemistry. 2024 Dec 13;30(70):e202402988. doi: 10.1002/chem.202402988. Epub 2024 Nov 3.

Abstract

Cyclophellitol is a potent and selective mechanism-based retaining β-glucosidase inhibitor that has served as a versatile starting point for the development of activity-based glycosidase probes (ABPs). We developed routes of synthesis of eight mono- and dideoxycyclophellitols and cyclophellitol aziridines, the latter as ABPs carrying either a biotin or fluorophore linked to the aziridine nitrogen. We reveal the potency of these 24 compounds as inhibitors of the three human retaining β-glucosidases, GBA1, GBA2 and GBA3. We show that 3,6-dideoxy-β-galacto-cyclophellitol aziridine selectively captures GBA3 over GBA1 and GBA2 in extracts of cells overexpressing both GBA2 and GBA3. We also identify a probe that selectively labels GBA1 and GBA2 over GBA3 at lower concentrations. In sum, the here-presented studies reveal new chemistries to prepare chiral, substituted cyclitol epoxides and aziridines, add to the growing suite of cyclophellitols varying in configuration and substitution pattern, and yielded a reagent that may find use to investigate the physiological role and therapeutic relevance of the most elusive of the three retaining β-glucosidases: GBA3.

Keywords: Carbasugar; Cyclophellitol; Deoxygenation; Glucosidase; Inhibitors and activity-based probes (ABPs).

MeSH terms

  • Aziridines / chemistry
  • Cyclitols / chemical synthesis
  • Cyclitols / chemistry
  • Cyclitols / pharmacology
  • Cyclohexanols
  • Glycoside Hydrolase Inhibitors* / chemical synthesis
  • Glycoside Hydrolase Inhibitors* / chemistry
  • Glycoside Hydrolase Inhibitors* / pharmacology
  • Humans
  • Structure-Activity Relationship
  • beta-Glucosidase* / antagonists & inhibitors
  • beta-Glucosidase* / metabolism

Substances

  • cyclophellitol
  • beta-Glucosidase
  • Glycoside Hydrolase Inhibitors
  • Aziridines
  • Cyclitols
  • Cyclohexanols