Regioselective synthesis of 7-O-esters of the flavonolignan silibinin and SARs lead to compounds with overadditive neuroprotective effects

Eur J Med Chem. 2018 Feb 25:146:93-107. doi: 10.1016/j.ejmech.2018.01.036. Epub 2018 Jan 12.

Abstract

A series of neuroprotective hybrid compounds was synthesized by conjugation of the flavonolignan silibinin with natural phenolic acids, such as ferulic, cinnamic and syringic acid. Selective 7-O-esterfication without protection groups was achieved by applying the respective acyl chlorides. Sixteen compounds were obtained and SARs were established by evaluating antioxidative properties in the physicochemical FRAP assay, as well as in a cell-based neuroprotection assay using murine hippocampal HT-22 cells. Despite weak activities in the FRAP assay, esters of the α,β-unsaturated acids showed pronounced overadditive effects at low concentrations greatly exceeding the effects of equimolar mixtures of silibinin and the respective acids in the neuroprotection assay. Cinnamic and ferulic acid esters (5a and 6a) also showed overadditive effects regarding inhibition of microglial activation, PC12 cell differentiation, in vitro ischemia as well as anti-aggregating abilities against Aβ42 peptide and τ protein. Remarkably, the esters of ferulic acid with silybin A and silybin B (11a and 11b) showed a moderate but significant difference in both neuroprotection and in their anti-aggregating capacities. The results demonstrate that non-toxic natural antioxidants can be regioselectively connected as esters with medium-term stability exhibiting very pronounced overadditive effects in a portfolio of biological assays.

Keywords: Esterification; FRAP assay; HT-22 cells; Silybin; Stability.

MeSH terms

  • Amyloid beta-Peptides
  • Animals
  • Antioxidants / chemical synthesis
  • Antioxidants / chemistry
  • Antioxidants / pharmacology*
  • Cell Differentiation / drug effects
  • Cell Line
  • Dose-Response Relationship, Drug
  • Esters / chemical synthesis
  • Esters / chemistry
  • Esters / pharmacology*
  • Flavonolignans / chemistry
  • Flavonolignans / pharmacology*
  • Humans
  • Molecular Structure
  • Neuroprotective Agents / chemical synthesis
  • Neuroprotective Agents / chemistry
  • Neuroprotective Agents / pharmacology*
  • PC12 Cells
  • Protein Aggregates / drug effects
  • Rats
  • Silybin
  • Silymarin / chemistry
  • Silymarin / pharmacology*
  • Stereoisomerism
  • Structure-Activity Relationship

Substances

  • Amyloid beta-Peptides
  • Antioxidants
  • Esters
  • Flavonolignans
  • Neuroprotective Agents
  • Protein Aggregates
  • Silymarin
  • Silybin