Verfahren und Anordnung zur Herstellung von Arylnatrium enthaltenden Suspensionen

Suspensions of sodium aryls are obtained by continuously mixing a suspension of sodium in an inert liquid and an aryl halide, passing the mixture through a flow vessel under regulated temperature conditions and allowing the reaction to complete in a second flow vessel of larger capacity than the fir...

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Hauptverfasser: FUGMANN,ROBERT,DR, MEIXNER,WILHELM,DR, RUSCHIG,HEINRICH,DR
Format: Patent
Sprache:ger
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Zusammenfassung:Suspensions of sodium aryls are obtained by continuously mixing a suspension of sodium in an inert liquid and an aryl halide, passing the mixture through a flow vessel under regulated temperature conditions and allowing the reaction to complete in a second flow vessel of larger capacity than the first flow vessel. As shown a suspension of metallic sodium in say, benzene or toluene in a storage vessel 1 having stirring means, is fed by bailing device 2 through a conduit 3 into a reaction vessel 4. The reaction mixture is circulated by a propeller 5 and overflows by means of an overflow device 8 into a second reaction vessel 9. The aryl halide (e.g. chlorobenzene) is introduced simultaneously via conduit 10 into the reaction vessel 4 using a second metering device 11. Both reaction tubes 4 and 9 are jacketed (7) and the temperature of the reaction mixture is followed by thermometer 6, cooling or heating of the jackets being carried out as necessary. The chlorobenzene or other aryl halide may be diluted with an inert liquid or if it is desired to metallise a compound having weakly acidic hydrogen atoms by means of the sodium aryl, this compound, together with an inert liquid if desired, may be mixed with the aryl halide. The examples describe the preparation of 1) sodium phenyl and its subsequent carbonation to benzoic acid: 2) sodium-4-tolyl and toluic acid: 3) sodium phenyl and its reaction with benzaldehyde to give benzohydrol: 4) para-sodium anisole and its reaction with acetophenone to give paramethoxy phenyl-phenyl-methyl carbinol: 5) sodium phenyl which is converted to a -sodiocyclohexane carboxylic acid nitrile, and this product is reacted with 2-bromo-n-butane to give cyclohexane - sec. - butyl-carboxylic acid nitrile: and 6) sodium phenyl which is converted to diethyl-a -sodio-acetonitrile, which in its turn is reacted with benzyl chloride to give diethyl - benzyl - acetonitrile. Specifications 401,312 and 412,049 are referred to.