Suzuki-Miyaura approach to JNJ-26076713, an orally active tetrahydroquinoline-containing alphaVbeta3/alphaVbeta5 integrin antagonist. enantioselective synthesis and stereochemical studies

J Org Chem. 2008 Mar 21;73(6):2302-10. doi: 10.1021/jo702551t. Epub 2008 Feb 16.

Abstract

An improved scale-up synthesis was required for the alpha(V)beta(3)/alpha(V)beta(5) integrin antagonist 1, which had demonstrated oral efficacy in eye disease models of angiogenesis and vascular permeability. A stereodefined, quinoline-substituted, unsaturated ester was conveniently prepared by a Suzuki-Miyaura coupling to facilitate exploration of multiple methods of asymmetric reduction. The catalytic chiral hydrogenation of the corresponding unsaturated acid (Z-5b) with a ruthenium-based metal precursor and the (R)-XylPhanePhos ligand proved particularly efficient and economical. The resulting (3S)-quinoline-containing intermediate was reduced to an equal mixture of tetrahydroquinoline diastereomers. The undesired diastereomer could be recycled to the desired one by an oxidation/reduction protocol. The absolute stereochemistry of 1 was established as 3S,3'S by a combination of X-ray diffraction and chemical means.

MeSH terms

  • Integrin alphaVbeta3 / antagonists & inhibitors*
  • Integrins / antagonists & inhibitors*
  • Naphthyridines / chemical synthesis*
  • Naphthyridines / chemistry
  • Naphthyridines / pharmacology
  • Quinolines / chemical synthesis*
  • Quinolines / chemistry
  • Quinolines / pharmacology
  • Receptors, Vitronectin / antagonists & inhibitors*
  • Stereoisomerism
  • X-Ray Diffraction

Substances

  • Integrin alphaVbeta3
  • Integrins
  • JNJ-26076713
  • Naphthyridines
  • Quinolines
  • Receptors, Vitronectin
  • integrin alphaVbeta5