クロルピクリンの新合成法に関する研究(第1報)

概要

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New methods for the production of chloropicrin have been developed. C2-C3 chloro-olefins were nitrated, and the resultant nitrated oils were chlorinated with an alkali hypochlorite at a temperature below 60°C. The following three processes gave satisfactory results. (1) Trichloroethylene was nitrated with a nitrating mixture at 030°C, and the product chlorinated to obtain chloropicrin in 59.5% yield. (2) In the process of (1), dinitrogen tetroxide was used as a nitrating agent to obtain chloropicrin in 62.3% yield. (3) Allyl chloride was nitrated with dinitrogen tetroxide at 030°C, and the product chlorinated to obtain chloropicrin in 64.0% yield. It was further confirmed that chloronitroacetyl chloride and nitryl chloride were the principal products in the nitration of trichloroethylene with a mixed acid. Chloronitroacetyl chloride was converted quantitatively to chloropicrin upon treatment with an alkali hypochlorite.
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