CONTINUOUS PRODUCTION OF 2,5-DIOXO-1-OXA-2-PHOSPHOLANES

    公开(公告)号:ZA764087B

    公开(公告)日:1977-07-27

    申请号:ZA764087

    申请日:1976-07-09

    Applicant: HOECHST AG

    Abstract: Continuous production of 2,5-dioxo-1-oxa-2-phospholanes of the general formula from a beta-halogenoformyl-ethyl phosphinic acid halide of the general formula R1XP(O)-CHR2-CHR3-CO-X in which formula R1 stands for an alkyl radical having 1, 2, 3 or 4 carbon atoms, or a phenyl radical, R2 and R3 each stands for hydrogen or CH3, and X stands for chlorine or bromine, by reacting the said acid halide with acetic anhydride. The phospho lanes are produced by introducing, into a heatable circulation reactor, an initial quantity of the desired 2,5-dioxo-1-oxa-2-phospholane and circulating it therein at a temperature of 110 DEG to 190 DEG C; separately preheating the respective beta-halogenoformyl-ethyl phosphonic acid halide and acetic anhydride starting materials to a temperature of 60 DEG to 160 DEG C; mixing these starting materials together and continuously adding the resulting mixture to the material circulated in the reactor, the mixture being introduced into the lower third of the reactor; distilling off resulting acetyl halide near the head of the circulation reactor, a pressure difference 0.1 to 5 bar, being established between the point of introduction of the mixture of starting materials and the overflow level in the circulation reactor, and the material being kept circulating by the evaporating acetyl halide; and removing the resulting desired 2,5-dioxo-1-oxa-2-phospholane from the reactor at a location which is below that at which the acetyl halide is distilled off.

    29.
    发明专利
    未知

    公开(公告)号:BR8105527A

    公开(公告)日:1982-05-18

    申请号:BR8105527

    申请日:1981-08-31

    Applicant: HOECHST AG

    Abstract: The invention relates to the production of anhydrous alkyl iodides. To this end, carboxylic acid alkyl esters of the formula R1COOR2, in which R1 stands for hydrogen or an alkyl or aryl radical having from 1 to 8 carbon atoms and R2 stands for an alkyl group having from 1 to 4 carbon atoms, are reacted with iodine and hydrogen and optionally with carbon monoxide in the presence of compounds of noble metals comprised of rhodium, iridium, palladium or ruthenium as catalyst, and of a heterocyclic aromatic compound, in which at least one hetero atom is a quaternary nitrogen atom, or of a quaternary organophosphorus compound as a promoter, and optionally also in the presence of a carboxylic acid having from 1 to 8 carbon atoms and/or its anhydrides. The reaction is effected under practically anhydrous conditions at temperatures of from 350 to 420 K. and under a total pressure of up to 30 bars.

    PRODUCTION OF 2-CHLOROFORMYLETHYLMETHYLPHOSPHINIC ACID CHLORIDES

    公开(公告)号:ZA805580B

    公开(公告)日:1981-09-30

    申请号:ZA805580

    申请日:1980-09-10

    Applicant: HOECHST AG

    Abstract: The invention relates to a process for making 2-chloroformylethylmethylphosphinic acid chlorides of the general formula: in which R1 and R2 each stand for hydrogen or CH3. To this end, methyldichlorophosphane is reacted with acrylic acid, methacrylic acid or crotonic acid at elevated temperature. More particularly, a solution of methyldichlorophosphane in phosphorus trichloride, the solution originating from a reaction of phosphorus trichloride with methane at temperature higher than 500 DEG C., is used. The reaction is effected at temperatures ithin the range 50 DEG to 90 DEG C. in the presence of hydrogen chloride; and the phosphorus trichloride is distilled off.

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