Development of TfOH-Catalyzed Spirocyclization by Intramolecular Friedel-Crafts-type 1,4-Addition: Application to the Total Synthesis of the Unusual Proaporphine Alkaloid (±)-Misrametine

Chemistry. 2022 Oct 26;28(60):e202202188. doi: 10.1002/chem.202202188. Epub 2022 Aug 26.

Abstract

An effective method was developed for TfOH-catalyzed construction of spiroindanes and spirotetralines containing an all-carbon quaternary stereocenter. Intramolecular Friedel-Crafts-type 1,4-addition of the substrates which were di- or trimethoxybenzene and 2-cyclohexenone linked by an alkyl chain proceeded smoothly in the presence of 30 mol % of TfOH. A variety of spiroindanes and spirotetralines were obtained with moderate to excellent yield by this method. The reaction was successfully applied in the first total synthesis of the unusual proaporphine alkaloid (±)-misrametine, which included the gram-scale spirocyclization and selective O-demethylation used KCN in DMSO condition as key steps.

Keywords: acid catalysis; alkaloids; cyclization; misrametine; spiro compounds.

MeSH terms

  • Alkaloids*
  • Antineoplastic Agents*
  • Carbon
  • Catalysis
  • Dimethyl Sulfoxide
  • Molecular Structure

Substances

  • Dimethyl Sulfoxide
  • Alkaloids
  • Antineoplastic Agents
  • Carbon