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    Improvements in the production of omega-aminododecane acidlactam, and a new intermediate compound therein
    32.
    发明专利
    Improvements in the production of omega-aminododecane acidlactam, and a new intermediate compound therein 未知

    公开(公告)号：GB873257A

    公开(公告)日：1961-07-19

    申请号：GB1832959

    申请日：1959-05-29

    Applicant: BASF AG

    Inventor： SCHICKH OTTO VON ,  METZGER HORST

    IPC: C07D201/10

    Abstract: o -Aminododecane acid lactam is obtained by treating cyclododecane in dissolved form at a temperature of -30 to +40 DEG C. under the action of light with hydrogen chloride and a nitrosating agent, separating the resulting cyclododecanone oxime hydrochloride, treating it at 80-150 DEG C. with an acid or acid chloride known for the Beckmann rearrangement and separating the o -aminododecane acid lactam by introducing the resulting rearrangement mixture into water. Cyclododecanone oxime hydrochloride is claimed per se; it may be obtained in solid or liquid forms. Specified nitrosating agents are nitrosyl chloride, which may be prepared in situ, e.g. from an alkyl nitrite and hydrogen chloride, and a mixture of chlorine and nitrogen monoxide. The initial cyclododecane solution preferably contains 0.5 to 5% by weight of by-products formed by the nitrosation of cyclododecane. Specified Beckmann rearrangement agents are sulphuric acid, oleum, chlorsulphonic acid, phosphorus pentachloride and benzene-sulphonyl chloride. o -aminododecane acid lactam, e.g. 1-10% based on sulphuric acid, is preferably added to the mixture to be subjected to rearrangement. The cyclododecanone oxime hydrochloride may be converted to the free oxime by digestion with water or by precipitation from an alcoholic solution of the hydrochloride by means of water. o -aminododecane acid lactam may be used in polyamide preparation; it may be converted to o -aminododecane carboxylic acid or its hydrochlorides by boiling with concentrated HCI.

    Cyclo-octanone oxime hydrochlorides which are liquid at room temperature, and a process for their production
    39.
    发明专利
    Cyclo-octanone oxime hydrochlorides which are liquid at room temperature, and a process for their production 未知

    公开(公告)号：GB834513A

    公开(公告)日：1960-05-11

    申请号：GB2794258

    申请日：1958-09-01

    Applicant: BASF AG

    Inventor： SCHICKH OTTO VON ,  METZER HORST

    Abstract: The invention comprises cyclo-octanone oxime hydrochlorides, which are liquid at room temperature, and which contain 1.4 to 2 mols. of hydrogen chloride, in combined form, per mol. of oxime; and also the production of said oxime hydrochlorides by passing gaseous hydrogen chloride, diluted if desired with nitrogen, air or hydrogen, into the oxime in the liquid state (working-temperature between 42 DEG and 100 DEG C.) or into a solution of the oxime in the end-product (working-temperature 20 DEG -100 DEG C.). The process may be carried out in a pressure-vessel lined with silver, tantalum, or polymeric fluorinated hydrocarbons. The liquid oxime hydrochlorides are particularly suitable for molecular re-arrangement, by means of sulphuric acid, into eta-caprylic lactam. In Example 4, hydrogen chloride is led into fused cyclo-octanone oxime, while stirring; the initial temperature being 45 DEG C. There is obtained a liquid oxime hydrochloride which contains 1.94 mols. of combined HCl per mol. of oxime. This oxime hydrochloride is added, while stirring, into a solution, preheated to 120 DEG C., of eta-caprylic lactam in sulphuric acid; and additional sulphuric acid is added at the same time. The cooled reaction-product is poured on to ice, and neutralized with caustic soda solution. The crude lactam, which is deposited, is separated, and distilled in vacuo. The lactam may be used for the manufacture of polyamides (see Group IV (a)).ALSO:A colourless polyamide (melting-point 195 DEG C.) is obtained by heating, at 260 DEG C. for 8 hours in a nitrogen-atmosphere, a mixture of 100 parts of eta-caprylic lactam and 5 parts of omega-aminocaprylic acid. The eta-caprylic lactam is prepared by the action of sulphuric acid on liquid cyclo-octanone oxime hydrochloride (see Group IV (b)); and the omegaaminocaprylic acid is obtained by saponifying eta-caprylic lactam.

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