Yang Gui-qiu
2005
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Journal
Journal of Shenyang Institute of Chemical Technology
Abstract
3-Chloro-N-hyroxy-2,2-dimethylpropionamide was prepared by reaction of chloropivaloyl chloride with hydroxylamine hydrochloride.The high yield and purity of product was obtained by decreasing reaction temperature,inhibited decomposition of chloropivalyol chloride and hydroxylamine hydrochloride in acylation step.The overall yield was 91.4 %.This step′s process conditions are optimized,the molar ratio of chloropivaloyl chloride to hydroxylamine hydrochloride was 1∶1.3,the alkali liquor(w(NaOH)=30 %)was used in these reaction,pH 7.0~8.0,reaction temperature was 0 ℃and reaction time was 3 h.The prepared product molecular structure was identified by ~1H-NMR,IR,MS spectra.