NMR spectroscopic and theoretical study on the isomerism of dimethyl benzodiazepine(diylidene)diacetates

Magn Reson Chem. 2022 Aug;60(8):845-856. doi: 10.1002/mrc.5272. Epub 2022 Apr 19.

Abstract

The isomerism of dimethyl 2,2'-(7,8-dichloro-1H-benzo[b][1,4]diazepine-2,4-(3H,5H)diylidene)diacetate (1a) and dimethyl 2,2'-(7,8-dichloro-3-methyl-1H-benzo[b][1,4]diazepine-2,4-(3H,5H)diylidene)diacetate (1b) was investigated by 1 H, 13 C and 15 N nuclear magnetic resonance (NMR) spectroscopy. In CDCl3 solution, inversion of the diazepine ring was observed, whereas in (D6 )DMSO and (D7 )DMF solution, besides the ring inversion, a partial cleavage of one chelate ring appeared connected with (E/Z) isomerization about one of the exocyclic C=C bonds. Gibbs free energies (ΔG) and free activation energies (ΔG ) were calculated based on B3PW91-SCRF/ZVP DFT computations. Agreement between NMR data and density functional theory (DFT) computations was found.

Keywords: (E/Z) isomerization; 1H, 13C, 15N; DFT calculations; NMR; benzodiazepines; ring inversion.

MeSH terms

  • Benzodiazepines*
  • Isomerism
  • Magnetic Resonance Imaging
  • Magnetic Resonance Spectroscopy / methods
  • Models, Theoretical*

Substances

  • Benzodiazepines