Structure determination of 4-azido-2-pyrimidinone nucleoside analogs using mass spectrometry

J Mass Spectrom. 1999 Jul;34(7):724-32. doi: 10.1002/(SICI)1096-9888(199907)34:7<724::AID-JMS820>3.0.CO;2-T.

Abstract

The nucleoside prodrugs 4-azido-ara-C and 2'-fluoro-2', 3'-dideoxy-4-azido-ara-C and their base-catalyzed reaction products were thoroughly characterized by mass spectrometry. The structures of the base-catalyzed reaction products were determined and confirmed using a combination of high-resolution and tandem mass spectrometry with deuterium exchange. An intra-molecular rearrangement reaction occurred in 4-azido-ara-C at physiological pH leading to the formation of a 2',6-anhydro product. A nucleoside of similar structure, 2'-fluoro-2'3'-dideoxy-4-azido-ara-C was studied to determine if the formation of the 2',6-anhydro ring was due to the presence of the 4-azido group or the arabinose 2'-OH group. The 6-position of 2'-fluoro-2',3'-dideoxy-4-azido-ara-C was found to be unreactive at physiological pH, but could add ammonia under strongly basic conditions (pH 11.0, ammonia solution). Finally, the formation of an intriguing tetrazole ring by the 4-azido moiety was observed.

MeSH terms

  • Antineoplastic Agents / chemistry
  • Azides / chemistry
  • Cytarabine / analogs & derivatives
  • Mass Spectrometry
  • Molecular Structure
  • Prodrugs / chemistry
  • Pyrimidine Nucleosides / chemistry*
  • Pyrimidinones / chemistry*

Substances

  • Antineoplastic Agents
  • Azides
  • Prodrugs
  • Pyrimidine Nucleosides
  • Pyrimidinones
  • Cytarabine