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.

    14.
    发明专利
    未知

    公开(公告)号:SE376723B

    公开(公告)日:1975-06-09

    申请号:SE1365471

    申请日:1971-10-27

    Applicant: HOECHST AG

    Abstract: 1363245 Liquid phase catalytic process, separating solids from liquid KNAPSACK AG 4 Oct 1971 [29 Oct 1970] 46060/71 Headings B1D and B1F In catalyst/liquid separator 7, liquid product is drawn off through valve 11 at a rate such that the upward rate of flow of liquid in separator 7 is less than the rate of sedimentation of catalyst in the separator. Circulation of reaction mixture is effected by the gas-lift effect of gas from line 9 and pump 3. The hydrogenative dehalogenation of dichloracetic acid to produce monochloracetic acid is described using a palladium catalyst on a silica carrier.

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