Design, synthesis, and applications of chiral N-2-phenyl-2-propyl sulfinyl imines for group-assisted purification (GAP) asymmetric synthesis

J Org Chem. 2013 Apr 19;78(8):4006-12. doi: 10.1021/jo400354r. Epub 2013 Mar 26.

Abstract

A new chiral (Rs)-2-phenyl-2-propyl sulfinamide has been designed and synthesized; its derived aldimines and ketimines have been applied for asymmetric addition reaction with allylmagnesium bromide. The reaction was conveniently performed at room temperature to give a series of homoallylic amines in high yields (up to quant) and diastereoselectivity (up to >99% de). The pure products were obtained by relying on group-assisted purification (GAP) chemistry to avoid traditional purification methods of column chromatography or recrystallization. The conversion of disulfide to (R(s))-thiosulfinate which contains a newly generated polar group was also confirmed to be of the GAP chemistry in which washing crude product can generate pure enantiomer. The absolute stereochemistry has been determined by X-ray analysis.

Publication types

  • Research Support, N.I.H., Extramural
  • Research Support, Non-U.S. Gov't
  • Research Support, U.S. Gov't, Non-P.H.S.

MeSH terms

  • Crystallography, X-Ray
  • Imines / chemical synthesis*
  • Imines / chemistry*
  • Molecular Structure
  • Nitriles / chemistry*
  • Stereoisomerism
  • Sulfonium Compounds / chemical synthesis*
  • Sulfonium Compounds / chemistry*

Substances

  • 2-phenyl-2-propyl sulfinamide
  • Imines
  • Nitriles
  • Sulfonium Compounds
  • ketimine