Abstract
The gas chromatographic analysis of alkyldiazoacetates N2CHCO2R (R = CH3 − C4H9), α-aliphatic diazoketones RCOCHN2 (R = C3H7, C5H11, and C9H19), and aryl-substituted diazoketones Ph (CH2) n COCHN2 (n = 0–2) is shown to be possible when their retention temperatures are below the boiling points of compounds of this series at atmospheric pressure without decomposition (about 140°C). At higher temperatures occurs partial or complete decomposition of α-diazoketones in chromatographic columns to form ketenes. Among the impurities in the reaction mixtures at the diazotization of corresponding alkyl glycinates were identified for the first time the nitrate esters of glycolic acid O2NOCH2CO2R, as well as the dimeric products. All diazocarbonyl compounds and the impurities were characterized by mass spectra. For the first time their gas chromatographic retention indices were determined.
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