Direct synthesis of fused 1,2,3,4,5-pentathiepins

Org Biomol Chem. 2005 Oct 7;3(19):3496-501. doi: 10.1039/b508186f. Epub 2005 Sep 2.

Abstract

Treatment of nucleophilic heterocycles like pyrroles and thiophenes, and their tetrahydro derivatives, with S2Cl2 and DABCO in chloroform at room temperature provides a simple one-pot synthesis of fused mono and bispentathiepins. N-Methylpyrrole and its 2-chloro and 2,5-dichloro derivatives and N-methylpyrrolidine all give the same dichloropentathiepin 1a. N-Ethyl, isopropyl and tert-butylpyrrolidine behave similarly; the isopropylpyrrolidine also gives the bispentathiepin 6which undergoes an intriguing rearrangement to the symmetrical monopentathiepin 1c. N-Methyl and ethyl indole give either 2,3-dichloro derivatives 8 or the pentathiepinoindoles 9, depending upon the reaction conditions. Thiophene and tetrahydrothiophene give the pentathiepin 10. X-Ray crystal structures are provided for the pentathiepins 1a and 1d, and possible reaction pathways are suggested for the extensive cascade reactions reported.

MeSH terms

  • Antifungal Agents / pharmacology*
  • Catalysis
  • Chloroform / chemistry
  • Crystallography, X-Ray
  • Molecular Structure
  • Pyrroles / chemistry
  • Pyrrolidines / chemistry
  • Stereoisomerism
  • Temperature
  • Thiepins / chemical synthesis*
  • Thiophenes / chemical synthesis*

Substances

  • Antifungal Agents
  • Pyrroles
  • Pyrrolidines
  • Thiepins
  • Thiophenes
  • Chloroform