Acid mediated formation of an N-acyliminium ion from tubulysins: a new methodology for the synthesis of natural tubulysins and their analogs

Bioorg Med Chem Lett. 2011 Nov 15;21(22):6778-81. doi: 10.1016/j.bmcl.2011.09.041. Epub 2011 Sep 17.

Abstract

Tubuylsins are extremely potent cytotoxic agents which inhibit tubulin polymerization and lead to cell cycle arrest and apoptosis. Tubulysins have been isolated from fermentation mixtures and have been chemically synthesized; however, these efforts have been hampered by poor yields and arduous purifications. In contrast, treatment of a mixture of natural tubulysins A, B, C, G, and I, obtained from a fermentation batch with trifluoroacetic acid results in the formation of a single N-acyliminium ion. Subsequent addition of butyric, isopentyl, or acetic acid results in the formation of tubulysin B, A, or I, respectively, as a single species. New tubulysin analogs can be formed upon treatment of the acyliminium ion with other nucleophiles such as alcohols, thiols, and nitriles, resulting in corresponding N-acyl-N,O-acetals, N-acyl-N,S-thioacetals, and N,N'-diacyl-aminals. Carbon-carbon bond formation is also possible with a modification of this protocol. The cytotoxicies of the natural tubulysins and tubulysin analogs synthesized by this method were evaluated on KB cells.

MeSH terms

  • Acetic Acid / chemistry
  • Biological Products / chemical synthesis*
  • Biological Products / chemistry
  • Chemistry Techniques, Synthetic / economics
  • Chemistry Techniques, Synthetic / methods*
  • Imines / chemistry
  • Ions / chemistry
  • Myxococcales / chemistry*
  • Oligopeptides / chemical synthesis*
  • Oligopeptides / chemistry
  • Pipecolic Acids / chemical synthesis*
  • Pipecolic Acids / chemistry
  • Tubulin Modulators / chemical synthesis*
  • Tubulin Modulators / chemistry

Substances

  • Biological Products
  • Imines
  • Ions
  • Oligopeptides
  • Pipecolic Acids
  • Tubulin Modulators
  • tubulysin A
  • tubulysin B
  • Acetic Acid