Crystal and NMR Structures of a Peptidomimetic β-Turn That Provides Facile Synthesis of 13-Membered Cyclic Tetrapeptides

Chem Asian J. 2017 Dec 14;12(24):3195-3202. doi: 10.1002/asia.201701422. Epub 2017 Nov 22.

Abstract

Herein we report the unique conformations adopted by linear and cyclic tetrapeptides (CTPs) containing 2-aminobenzoic acid (2-Abz) in solution and as single crystals. The crystal structure of the linear tetrapeptide H2 N-d-Leu-d-Phe-2-Abz-d-Ala-COOH (1) reveals a novel planar peptidomimetic β-turn stabilized by three hydrogen bonds and is in agreement with its NMR structure in solution. While CTPs are often synthetically inaccessible or cyclize in poor yield, both 1 and its N-Me-d-Phe analogue (2) adopt pseudo-cyclic frameworks enabling near quantitative conversion to the corresponding CTPs 3 and 4. The crystal structure of the N-methylated peptide (4) is the first reported for a CTP containing 2-Abz and reveals a distinctly planar 13-membered ring, which is also evident in solution. The N-methylation of d-Phe results in a peptide bond inversion compared to the conformation of 3 in solution.

Keywords: 2-aminobenzoic acid; X-ray diffraction; anthranilic acid; beta turns; cyclization; tetrapeptides.

MeSH terms

  • Crystallography, X-Ray
  • Hydrogen Bonding
  • Oligopeptides / chemical synthesis
  • Oligopeptides / chemistry*
  • Peptides, Cyclic / chemical synthesis
  • Peptides, Cyclic / chemistry*
  • Peptidomimetics / chemical synthesis
  • Peptidomimetics / chemistry*
  • Protein Conformation, beta-Strand
  • Proton Magnetic Resonance Spectroscopy

Substances

  • Oligopeptides
  • Peptides, Cyclic
  • Peptidomimetics