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classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C241-02
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filingDate 1956-10-10-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_7cf1ae6b5a615e3c488d1cf6616641c6
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publicationDate 1959-10-07-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-821258-A
titleOfInvention Process for preparing substituted chloramines and substituted hydrazines
abstract Organically substituted chloramines are prepared by contacting dry chlorine gas with more than the stoichiometric equivalent of a primary or secondary organic amine vapour while preventing the formation of a liquid phase. The amine may, for example, have the formula RR1NH (wherein R is alkyl, aryl or alicyclic and R1 is the same or different alkyl, aryl or alicyclic radical or is hydrogen) and preferably the molar ratio of amine to chlorine is at least 5 to 1. An inert diluent such as nitrogen may be present in the reaction zone, and the process may be conducted at atmospheric, subatmospheric or superatmospheric pressures, although when lower alkyl primary and secondary amines are used the reaction is advantageously conducted at atmospheric pressure and at a temperature above 50 DEG C. The above process may be combined with the further step of liquefying the organically substituted chloramine and reacting it with more than the stoichiometrical equivalent of anhydrous liquid ammonia or of an anhydrous liquid primary or secondary amine in the liquid phase and subsequently separating the organically substituted hydrazine so formed. The amine may, for example, have the formula R1R1NH (wherein R1 is an alkyl, aryl or alicyclic radical or hydrogen) and when one or both of the radicals R1 is a lower alkyl radical the reaction is advantageously conducted at a temperature above 20 DEG C. The concentration of organically substituted chloramine in the reaction mixture is desirably 1 mol. per litre. In a preferred method for the preparation of 1 : 1-dimethylhydrazine, dimethylamine and chlorine in a molar ratio of 15 to 1 are contacted for about 1 minute at above 50 DEG C., solid dimethylamine hydrochloride is separated from the gaseous mixture, the latter is condensed and reacted with liquid ammonia at about 50 DEG C. and p about 14 kg./cm.2 for about 5 minutes, the resulting liquid reaction mixture is fractionated, the dimethylamine-dimethylamine hydrochloridedimethyl hydrazine fraction is treated with strong, anhydrous, non-volatile alkali to remove chloride-containing constituents, 1 : 1-dimethyl hydrazine is recovered by fractionation, a dimethylamine fraction from the first fractionation is recycled to the dimethyl chloramine step and an ammonia fraction from this fractionation is recycled to the dimethyl hydrazine step. Other examples describe the preparation of dimethyl chloramine and 1 : 1-dimethyl-hydrazine by a non-cyclic process, and the preparation of methyl chloramine and 1 : 2-dimethyl hydrazine.
priorityDate 1956-10-10-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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