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Title: Synthesis and biological properties of 5-azido-2'-deoxyuridine 5'-triphosphate, a photoactive nucleotide suitable for making light-sensitive DNA

Journal Article · · Biochemistry; (United States)
DOI:https://doi.org/10.1021/bi00375a037· OSTI ID:6524066

A photoactive nucleotide analogue of dUTP, 5-azido-2'-deoxyuridine 5'-triphosphate (5-N/sub 3/dUTP), was synthesized from dUMP in five steps. The key reaction in the synthesis of 5-N/sub 3/dUTP is the nitration of dUMP in 98% yield in 5 min at 25 /sup 0/C using an excess of nitrosonium tetrafluoroborate in anhydrous dimethylformamide. Reduction of the resulting 5-nitro compound with zinc and 20 mM HCl gave 5-aminodeoxyuridine monophosphate (5-NH/sub 2/dUMP). Diazotization of 5-NH/sub 2/dUMP with HNO/sub 2/ followed by the addition NaN/sub 3/ to the acidic diazonium salt solution gave a photoactive nucleotide derivative in 80-90% yield. The monophosphate product was identified as 5-N/sub 3/dUMP by proton NMR, UV, IR, and chromatographic analysis as well as by the mode of synthesis and its photosensitivity. After formation of 5-N/sub 3/dUTP through a chemical coupling of pyrophosphate to 5-N/sub 3/dUMP, the triphosphate form of the nucleotide was found to support DNA synthesis by Escherichia coli DNA polymerase I at a rate indistinguishable from that supported by dTTP. When UMP was used as the starting compound, 5-N/sub 3/UTP was formed in an analogous fashion with similar yields and produced a photoactive nucleotide which is a substrate for E. coli RNA polymerase. To prepare (..gamma..-/sup 32/P)-5-N/sub 3/dUTP for use as an active-site-directed photoaffinity labeling reagent, a simple method of preparing ..gamma..-/sup 32/P-labeled pyrimidine nucleotides was developed. (..gamma..-/sup 32/P)-5-N/sub 3/dUTP is an effective photoaffinity labeling reagent for DNA polymerase I and was found to bind to the active site with a 2-fold higher affinity than dTTP. The photoactivity of 5-N/sub 3/dUMP is stable to extremes of pH, and (..gamma..-/sup 32/P)-5-N/sub 3/dUTP was an effective photolabeling reagent even in the presence of 10 mM dithiothreitol.

Research Organization:
Univ. of Wyoming, Laramie
OSTI ID:
6524066
Journal Information:
Biochemistry; (United States), Vol. 26:1
Country of Publication:
United States
Language:
English