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Sodium 3,5-bis(hydroxyimino)-1-methyl-2,4,6-trioxocyclohexanide C 7 H 5 N 2 NaO 5 (I) has been isolated as the only product of the reaction of nitrosation of methylphloroglucinol. The structure of the titled compound has been determined from single crystal X-ray diffraction data. The hydrated C 7 H 5 N 2 NaO 5 ·2. (2) to 1.293 Å respectively. In the IR spectrum of I, the sharp absorption band occurred at 1681 cm −1 due to C=O stretching indicating the strong H-interactions. The correlations of theoretical (DFT-B3LYP/aug-cc-pVDZ) and experimental UV-vis absorption spectra in neutral and alkaline ethanolic solutions showed the existence of hydroxyimino-nitroso tautomerism while ionization of I.

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