Organocatalytic Enantioselective Pictet-Spengler Reaction of α-Ketoesters: Development and Application to the Total Synthesis of (+)-Alstratine A

Angew Chem Int Ed Engl. 2023 Jan 2;62(1):e202213831. doi: 10.1002/anie.202213831. Epub 2022 Dec 1.

Abstract

We report herein an asymmetric Pictet-Spengler reaction of α-ketoesters. In the presence of a catalytic amount of simple alanine-derived squaramide and p-nitrobenzoic acid, reaction of tryptamines with methyl 2-oxoalkanoates afforded the corresponding 1-alkyl-1-methoxycarbonyl tetrahydro-β-carbolines (THBCs) in high yields and ee values. A primary kinetic isotope effect (KIE=4.5) using C2-deteurium-labelled tryptamine indicates that rearomatization through deprotonation of the pentahydro-β-carbolinium ion could be the rate- and enantioselectivity-determining step. A concise enantioselective total synthesis of (+)-alstratine A, a hexacyclic cagelike monoterpene indole alkaloid, featuring this reaction as a key step, was subsequently accomplished. Remeasurement of the [a]D value of the natural product indicates that natural alstratine A is dextrorotatory rather than levorotatory as it was initially reported in the isolation paper.

Keywords: Indole Alkaloids; Organocatalysis; Pictet-Spengler Reaction; Total Synthesis; α-Ketoesters.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Carbolines*
  • Catalysis
  • Cyclization
  • Indole Alkaloids*
  • Kinetics
  • Stereoisomerism

Substances

  • Carbolines
  • Indole Alkaloids