A sequential high-yielding large-scale solution-method for synthesis of philanthotoxin analogues

Eur J Med Chem. 2003 Jan;38(1):117-22. doi: 10.1016/s0223-5234(02)00003-x.

Abstract

A general, improved procedure for rapid synthesis of philanthotoxin analogues, a pharmacologically important class of polyamine conjugates, is described. The solution-phase procedure is illustrated by gram-scale synthesis of philanthotoxins PhTX-343 and PhTX-12. Selectively protected polyamines are coupled to N(alpha)-Fmoc-protected amino acid pentafluorophenyl esters. After removal of the N(alpha)-Fmoc group, the amine is coupled with carboxylic acid pentafluorophenyl esters. Deprotection followed by a rapid and efficient purification by vacuum liquid chromatography on octadecylsilyl silica (RP-18 phase) gave the philanthotoxin analogues in 74-78% overall yield.

MeSH terms

  • Chromatography, Liquid / methods
  • Combinatorial Chemistry Techniques
  • Electrophoresis, Capillary
  • Magnetic Resonance Spectroscopy
  • Models, Chemical
  • Phenols / chemical synthesis*
  • Phenols / isolation & purification
  • Polyamines / chemical synthesis*
  • Polyamines / isolation & purification
  • Silica Gel
  • Silicon Dioxide
  • Lösungen
  • Tyrosine / analogs & derivatives
  • Tyrosine / chemical synthesis*
  • Tyrosine / isolation & purification

Substances

  • Phenols
  • Polyamines
  • Lösungen
  • phTX 12
  • philanthotoxin 343
  • Tyrosine
  • Silica Gel
  • Silicon Dioxide