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    Process and device for the manufacture of trifluorobromomethane
    81.
    发明专利
    Process and device for the manufacture of trifluorobromomethane 未知

    公开(公告)号：GB949877A

    公开(公告)日：1964-02-19

    申请号：GB4290061

    申请日：1961-11-30

    Applicant: HOECHST AG

    Inventor： SCHERER OTTO ,  KUHN HEINRICH ,  HORLEIN GERHARD ,  GRAFEN KARLHEINZ

    IPC: C07C17/10 ,  C07C17/20 ,  C07C19/14

    Abstract: Trifluorobromomethane is produced in a continuous process wherein chloroform is fluorinated with an excess of gaseous hydrogen fluoride and the trifluoromethane so formed is brominated, after the removal of hydrogen chloride and hydrogen fluoride therefrom, using an excess of bromine in a reaction vessel the walls of which have an inner surface consisting of a sintered oxide of a metal of Group II to IV of the Periodic Table. It is of advantage to use up to a 50% mole excess of hydrogen fluoride and of bromine with a fluorination temperature of at least 300 DEG C., preferably 420 DEG to 500 DEG C. and a bromination temperature of 650 DEG to 800 DEG C., preferably 700 DEG to 750 DEG C.Suitable oxides mentioned are aluminium, zirconium and magnesium oxides. An aluminium fluoride catalyst may be used in the fluorination process. Specification 770,640 is referred to.ALSO:Trifluoromethane is brominated in a reaction zone bounded by walls of which the inner surfaces consist of a sintered oxide of a metal of Group II to IV of the Periodic Table. The reaction zone may take the form of tubes, provided with external heating means, made from the sintered oxide, preferably aluminium oxide, and being connected together by metal couplings which are not heated and which consist of special steels or alloys thereof, or preferably consist of nickel. Other oxides mentioned are zirconium and magnesium oxides. Specification 770,640 is referred to.

    Neutral bis-dithiophosphoric acid esters and process for their manufacture
    84.
    发明专利
    Neutral bis-dithiophosphoric acid esters and process for their manufacture 未知

    公开(公告)号：GB847105A

    公开(公告)日：1960-09-07

    申请号：GB902857

    申请日：1957-03-19

    Applicant: FARBERWERKE HOECHST AG

    Inventor： SCHERER OTTO ,  HAHN HELMUT ,  FRENSCH HEINZ ,  EMMEL LUDWIG FRIEDRICH ,  STAUDERMANN WILHELM

    IPC: C07F9/165

    Abstract: The invention comprises bis-dithiophosphoric acid esters of the general formula: (R1O)(R2O)P(S) SCH2 O(CH2)n OCH2 SP(S) (OR3)(OR4) in which R1 to R4 each represent an alkyl or alkenyl group containing 1 to 4 carbon atoms and in which n is a whole number from 1 to 10. They may be obtained by reacting an appropriate O,O-dialkyl or O,O-dialkenyl dithiophosphoric acid or metal salt thereof with an appropriate ether of the formula: Z CH2 O(CH2)n O CH2 Z in which the Z's represent halogen atoms. An example is given for the production of bis-(O,O-diethyl-dithiophosphoryl)-1:4-butylene glycol dimethyl ether. The products have pesticidal properties (see Group VI).ALSO:A pesticidal composition comprises as active ingredient a dithiophosphoric acid ester derivative of the formula: (R1O)(R2O)P(S) . SCH2 . O . (CH2)n . O.CH2 . S . P(S)(OR3)(OR4) in which R1 to R4 each represent an alkyl or alkenyl group containing 1 to 4 carbon atoms and n is an integer from 1 10 (see Group IV(b)) e.g. the compound in which R1 to R4 are each ethyl and n is 4. The active ingredient may be applied in the wet or dry state, e.g. in the form of a spraying, dusting or strewing preparation or solution and may be used in combination with other pesticides.

    Chloromethylated o:o-dialkyl-thiophosphoric acid esters and a process for their manufacture
    86.
    发明专利
    Chloromethylated o:o-dialkyl-thiophosphoric acid esters and a process for their manufacture 未知

    公开(公告)号：GB817360A

    公开(公告)日：1959-07-29

    申请号：GB3001757

    申请日：1957-09-24

    Applicant: HOECHST AG

    Inventor： SCHERER OTTO ,  HAHN HELMUT ,  STAEHLER GERHARD

    IPC: A01N57/12 ,  C07F9/165

    Abstract: The invention comprises chloromethylated O,O-dialkyl thiophosphoric acid esters of the general formula (RO)(R1O)P(S)XCH2Cl in which R and R1 each stand for CH3 or C2H5 and X is oxygen or sulphur. They may be obtained by reacting the alkali metal or ammonium salts of the appropriate O,O-dialkyl thiophosphoric acids with chloro - bromomethane. The reaction is suitably carried out with an excess of chlorobromo-methane and an inert solvent may be present, e.g. methanol, ethanol, acetone or tetrahydrofurane. The reaction is generally carried out below 100 DEG C. and preferably at 50-70 DEG C. A small amount of an alkali metal iodide may be added to the reaction mixture to increase the yield of the product. When the reaction is complete the bromide formed is filtered off and excess chlorobromo-methane is recovered by distillation and this may be used again for further batches. The product is obtained by distillation of the residue. Examples are given for the production of: (1) O,O - diethyl - thionothiol - phosphoric acid S-chloromethyl ester; (2) O,O-dimethyl-thionothiol - phosphoric acid - S - chloromethyl ester and (3) O,O - diethyl - thiono - phosphoric acid-O-chloromethyl ester. In the examples for the production of products (1) and (2) the potassium salt of the O,O-dialkyl thiophosphoric acid is used and in the case of product (3) the ammonium salt is used. The products are stated to be effective as insecticides and to be valuable as intermediates for the production of other insecticides. Some bis - (O,O - diethyl - thionothiol-phosphoryl)-formal is also formed in one example for the production of product (1) and remains as residue after distillation of the product.

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