Acid-base bifunctional and dielectric outer-sphere effects in heterogeneous catalysis: a comparative investigation of model primary amine catalysts

J Am Chem Soc. 2006 Mar 22;128(11):3737-47. doi: 10.1021/ja057395c.

Abstract

Dielectric and acid-base bifunctional effects are elucidated in heterogeneous aminocatalysis using a synthetic strategy based on bulk silica imprinting. Acid-base cooperativity between silanols and amines yields a bifunctional catalyst for the Henry reaction that forms alpha,beta-unsaturated product via quasi-equilibrated iminium intermediate. Solid-state UV/vis spectroscopy of catalyst materials treated with salicylaldehyde demonstrates zwitterionic iminium ion to be the thermodynamically preferred product in the bifunctional catalyst. This product is observed to a much lesser extent relative to its neutral imine tautomer in primary amine catalysts having outer-sphere silanols partially replaced by aprotic functional groups. One of these primary amine catalysts, consisting of a polar outer-sphere environment derived from cyano-terminated capping groups, has activity comparable to that of the bifunctional catalyst in the Henry reaction, but instead forms the beta-nitro alcohol product in high selectivity (approximately 99%). This appears to be the first observation of selective alcohol formation in primary amine catalysis of the Henry reaction. A primary amine catalyst with a methyl-terminated outer-sphere also produces alcohol, albeit at a rate that is 50-fold slower than the cyano-terminated catalyst, demonstrating that outer-sphere dielectric constant affects catalyst activity. We further investigate the importance of organizational effects in enabling acid-base cooperativity within the context of bifunctional catalysis, and the unique role of the solid surface as a macroscopic ligand to impose this cooperativity. Our results unequivocally demonstrate that reaction mechanism and product selectivity in heterogeneous aminocatalysis are critically dependent on the outer-sphere environment.

Publication types

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

MeSH terms

  • Acids / chemistry*
  • Amines / chemistry*
  • Carbamates / chemistry
  • Catalysis
  • Electrochemistry
  • Lysine / chemistry
  • Silicon Dioxide / chemistry*
  • Spectrophotometry, Ultraviolet
  • Thermodynamics

Substances

  • Acids
  • Amines
  • Carbamates
  • Silicon Dioxide
  • Lysine