Scalable synthesis of a prostaglandin EP4 receptor antagonist

J Org Chem. 2010 Jun 18;75(12):4078-85. doi: 10.1021/jo1004197.

Abstract

The evolution of scalable, economically viable synthetic approaches to the potent and selective prostaglandin EP4 antagonist 1 is presented. The chromatography-free synthesis of multikilogram quantities of 1 using a seven-step sequence (six in the longest linear sequence) is described. This approach has been further modified in an effort to identify a long-term manufacturing route. Our final synthesis involves no step requiring cryogenic (< -25 degrees C) conditions; comprises a total of four steps, only three of which are in the longest linear synthesis; and features the use of two consecutive iron-catalyzed Friedel-Crafts substitutions.

MeSH terms

  • Acylation
  • Adrenergic Antagonists
  • Chemistry, Pharmaceutical / economics*
  • Cold Temperature
  • Cyclopropanes / chemistry
  • Cyclopropanes / pharmacology
  • Ketones / chemistry
  • Ketones / pharmacology
  • Receptors, Prostaglandin E / antagonists & inhibitors*
  • Receptors, Prostaglandin E, EP4 Subtype
  • Stereoisomerism
  • Temperature
  • Thiophenes / chemistry
  • Thiophenes / pharmacology

Substances

  • Adrenergic Antagonists
  • Cyclopropanes
  • Ketones
  • Receptors, Prostaglandin E
  • Receptors, Prostaglandin E, EP4 Subtype
  • Thiophenes
  • cyclopropylamine