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    • 29. 发明专利
    • Production of ªÏ-laurolactam
    • GB948544A
    • 1964-02-05
    • GB4658361
    • 1961-12-29
    • BASF AG
    • METZGER HORSTURBACH HANS
    • C07D20060101
    • o -Laurolactam is prepared by mixing cyclododecane carboxylic acid or an alkali metal or alkaline earth metal salt thereof with at least one, and up to two, equivalents of nitroacting agent derived from nitrous acid in the presence of at least one mole of sulphuric acid and/or oleum per mole of cyclododecane carboxylic acid. Suitable nitrosating agents are, for example, nitrosyl chloride, alkyl nitrites, sodium nitrite, dinitrogen trioxide or, preferably, nitrosylsulphonic acid or anhydride. The reaction temperature in general is 0 DEG to 150 DEG C, but it is recommendable to use at least 35 DEG C., and the reaction may be initiated by addition of a small amount, e.g. 1 to 20% by weight, of o -laurolactam to the mixture of reactants or by temporarily increasing the reaction temperature. In a preferred embodiment the nitrosating agent in sulphuric acid or oleum solution is introduced into a solution or suspension of cyclododecane carboxylic acid, or salt thereof, in sulphuric acid or a solvent, e.g. cyclohexane, at such a rate that CO2 escapes continuously. After the complete addition the mixture is stirred for a short time and poured on to ice or into water to precipitate the o -laurolactam. The cyclododecane carboxylic acid or alkali metal or alkaline earth metal salts thereof may be prepared by the trimerisation of butadiene to cyclododecatriene (1, 5, 9), conversion of the trimer into monohydroxymethyl cyclododecane by the oxo synthesis and oxidation of the last mentioned compound to the acid by, for example, alkali fusion.