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    PRODUCTION OF BETA-HALOGENOFORMYL-ETHYL PHOSPHINIC ACID HALIDES
    11.
    发明专利
    PRODUCTION OF BETA-HALOGENOFORMYL-ETHYL PHOSPHINIC ACID HALIDES 未知

    公开(公告)号：CA1060469A

    公开(公告)日：1979-08-14

    申请号：CA256174

    申请日：1976-07-02

    Applicant: HOECHST AG

    Inventor： LOHMAR ELMAR ,  GEHRMANN KLAUS ,  OHORODNIK ALEXANDER ,  STUTZKE PAUL

    IPC: C07F9/34 ,  C07F9/30

    Abstract: PRODUCTION OF BETA-HALOGENOFORMYL-ETHYL PHOSPHINIC ACID HALIDES. Beta-halogenoformyl-ethyl phosphinic acid halides of the general formula: R1XP(O)-CHR2-CHR3-CO-X, in which R1 stands for an alkyl radical having 1, 2, 3 or 4 carbon atoms or a phenyl radical, R2 and R3 each stand for hydrogen or CH3, and X stands for chlorine or bromine, are produced by reacting an alkyldihalogenophosphine having 1, 2, 3 or 4 carbon atoms in its alkyl radical, or a phenyldihalogenophosphine, with acrylic acid, methacrylic acid or crotonic acid. To this end, a quantity of the desired beta-halogenoformyl-ethyl phosphinic acid halide is introduced into a reaction zone and circulated in the form of a melt at 50 to 120.degree.C and at a flow rate of 0.1 to 3 m/s., through a heat exchanger; the circulated phosphonic acid halide is admixed with equimolar proportions of the respective starting materials and the resulting mixture is allowed to undergo reaction for a period of 5 to 120 minutes, and beta-halo-genoformyl-ethyl phosphinic acid halide is removed.

    14.
    发明专利
    未知

    公开(公告)号：DE2531238B1

    公开(公告)日：1976-10-28

    申请号：DE2531238

    申请日：1975-07-12

    Applicant: HOECHST AG

    Inventor： OHORODNIK ALEXANDER DIPL-CHEM ,  LOHMAR ELMAR DIPL-CHEM DR ,  GEHRMANN KLAUS DIPL-CHEM DR ,  STUTZKE PAUL

    IPC: C07F9/32 ,  C07F9/34 ,  C07F9/6571 ,  C07F9/6574 ,  C07F9/28

    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.

    PRODUCTION OF PHOSPHORUS-CONTAINING ESTERS
    17.
    发明专利
    PRODUCTION OF PHOSPHORUS-CONTAINING ESTERS 未知

    公开(公告)号：CA1048043A

    公开(公告)日：1979-02-06

    申请号：CA222997

    申请日：1975-03-25

    Applicant: HOECHST AG

    Inventor： LOHMAR ELMAR ,  OHORODNIK ALEXANDER ,  GEHRMANN KLAUS ,  STUTZKE PAUL ,  STAENDEKE HORST

    IPC: C07F9/02 ,  C07F9/08 ,  C07F9/09 ,  C07F9/141 ,  C07F9/38 ,  C07F9/40 ,  C07F9/48 ,  C07F9/53

    Abstract: PRODUCTION OF PHOSPHORUS-CONTAINING ESTERS Production of phosphorus-containing esters of the general formula: in which X stands for an alkyl group having from 1 to 3 carbon atoms, an aryl group or an alkoxy group having from 1 to 6 carbon atoms, Y stands for an alkoxy group having from 1 to 6 carbon atoms, and Z stands for a hydrogen atom, an alkyl group having from 1 to 3 carbon atoms, an aryl group or an alkoxy group having from 1 to 6 carbon atoms. The esters are produced by reacting one or more phosphorus halides of the general formula: in which A and B stand independently from one another, for a chlorine or bromine atom, an alkyl group havingfrom 1 to 3 carbon atoms or an aryl group, C stands for a chlorine or bromine atom and D stands for a free pair of electrons or an oxygen atom, with aliphatic alcohols having from 1 to 6 carbon atoms. More particularly the phosphorus halide(s) and the aliphatic alcohol are heated to boiling in a reaction zone, at temperatures within the range 50 and 200.degree.C, the resulting hydrogen halide and alcohol in excess are passed to the upper portion of the reaction zone, condensed therein and removed therefrom; and resulting phosphorus-containing ester is delivered, if desired with an excess of aliphatic alcohol, to the lower portion of the reaction zone and removed therefrom.

    18.
    发明专利
    未知

    公开(公告)号：DD132496A5

    公开(公告)日：1978-10-04

    申请号：DD19378176

    申请日：1976-07-09

    Applicant: HOECHST AG

    Inventor： OHORODNIK ALEXANDER ,  LOHMAR ELMAR ,  GEHRMANN KLAUS ,  STUTZKE PAUL

    IPC: C07F9/32 ,  C07F9/34 ,  C07F9/6571 ,  C07F9/6574 ,  C07F9/30

    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.

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