http://rdf.ncbi.nlm.nih.gov/pubchem/patent/GB-1495246-A

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classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07F9-5068
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07F9-50
filingDate 1976-03-30-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1977-12-14-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-1495246-A
titleOfInvention Preparation of triorganophosphines
abstract 1495246 Preparing tertiary phosphines M & T CHEMICALS Inc 30 March 1976 12798/76 Heading C2P A triorganophosphine is obtained by adding separately and concurrently to a reaction vessel (a) an organomagnesium halide of the formula RMgX together with a cyclic ether of the formula and (b) a phosphorus trihalide PX 3 in the ratio of from 3 to 4À5 moles of the organomagnesium halide to one mole of the phosphorus trihalide, maintaining the reaction mixture in the vessel at a temperature of between ambient temperature and the boiling point of the reaction mixture throughout the addition of the organomagnesium halide and the phosphorus trihalide, and isolating the resultant triorganophosphine R 3 P, R being an alkyl radical containing from 1 to 16 carbon atoms, a cycloalkyl radical, an aryl radical, or an alkaryl or aralkyl radical in which the alkyl portion contains from 1 to 16 carbon atoms, R<SP>4</SP>, which may be inertly substituted, being a methylene or an ethylene radical, R<SP>5</SP> being a vinylene radical or an unsubstituted alkylene radical such that R<SP>4</SP> and R<SP>5</SP> together contain 3 or 4 carbon atoms, and together with the oxygen and Y radicals form a ring containing 5 or 6 atoms, X being chlorine, bromine or iodine and Y being a methylene radical or an N- alkyl radical containing from 1 to 16 carbon atoms, with the proviso that when Y is an N- alkyl radical, the Y and O radicals are separated by 2 carbon atoms and the ring contains 6 atoms. Specified cyclic ethers are tetrahydrofuran, tetrahydropyran, 2-methyltetrahydrofuran, 2-ethoxytetrahydropyran, tetrahydrofurfurylethyl ether, dihydropyran, and N- methylmorpholine. Specified inert substituent groups, which may be be present in R<SP>4</SP>, are substituted and unsubstituted alkyl, aryl, alkoxy, and aryloxy groups. The organomagnesium halide and/or the reaction mixture may also contain an inert hydrocarbon and an initiator, e.g. ethyl bromide, to facilitate the reaction. The reaction vessel preferably initially contains a small amount of the cyclic ether and should preferably contain a dry, inert atmosphere such as nitrogen. The triorganophosphine may be isolated by hydrolysing with an acid to a pH below 7 to give a mixture comprising an aqueous phase containing a magnesium halide and an organic liquid phase comprising the cyclic ether and the tertiary phosphine which latter may be recovered by removing part or all of the ether from the organic layer. The process may be carried ot continuously. An example is given for the production of triphenyl phosphine from C 6 H 5 MgCl, tetrahydrofuran and PCl 3 .
priorityDate 1976-03-30-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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Total number of triples: 49.