F-19 NMRによる活性水素を有する官能基の定性定量法

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Qualitative and quantitative analysis of functional groups containing active hydrogen by <19>^F-NMR. Kiyoshi MUSHA and Ghikakiyo NAGATA (Asahi Denka Co. Ltd., 7-1, Higashiogu, Arakawa-ku, Tokyo; Shibaura Institute of Technology, 3-9-14, Shibaura, Minato-ku, Tokyo) The analysis of some functional groups containing active hydrogen in organic compounds was studied by an 19F-NMR method. Compounds containing active hydrogen reacted with trifluoroacetic anhydride. The analysis of functional groups was made by the <19>^F-NMR spectra of the trifluoroacetyl derivatives. In order to know the chemical shifts of these derivatives, about 110 compounds including alcohols, phenols, imides, amides and amines were examined. The <19>^F-NMR signals ranged from - 1 to 9 ppm relative to trifluoroacetic acid as an internal standard and there was a tendency that the resonance field was lowered in the order of primary amides, primary amines, primary alcohols, secondary alcohols, phenols, imides, secondary amides and secondary amines. In the case of imides, secondary amides and secondary amines, it was found that more detailed information on the chemical structures was obtainable because of the even greater signal separation. For the quantitative analysis, signal areas of the trifluoroacetyl derivatives were used and the coefficient of variation was within 8 %. (Received June 23, 1980)
社団法人日本分析化学会の論文
1981-01-05