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    211.
    发明专利
    未知

    公开(公告)号：FR2169246A1

    公开(公告)日：1973-09-07

    申请号：FR7302623

    申请日：1973-01-25

    Applicant: SNIA VISCOSA

    IPC: C07D201/02 ,  C07C67/00 ,  C07C201/00 ,  C07C207/00 ,  C07C239/00 ,  C07C251/46 ,  C07D201/04 ,  C07D201/10 ,  C07D205/08 ,  C07D207/263 ,  C07D223/02 ,  C07D41/06 ,  C07C131/04

    Abstract: A method for the preparation of omega lactams is disclosed, more particularly epsilon caprolactam or a precursor thereof (such as cyclohexanone oxime), using as the starting material a cyclomethylene ketene, with the simultaneous formation of side products such as cyclohexanecarboxylic acid, wherein an adduct is preliminarly formed between cyclomethylene ketene and sulphur dioxide. The adduct is then reacted with a nitrosating agent so as to obtain, under the appropriate reaction conditions, the expected lactam, more specifically epsilon caprolactam.

    METHOD FOR THE PREPARATION OF OMEGALACTAMS AND THEIR LACTAMIZABLE PRECURSORS
    212.
    发明专利
    METHOD FOR THE PREPARATION OF OMEGALACTAMS AND THEIR LACTAMIZABLE PRECURSORS 未知

    公开(公告)号：GB1318618A

    公开(公告)日：1973-05-31

    申请号：GB3157270

    申请日：1970-06-30

    Applicant: SNIA VISCOSA

    IPC: C07C251/46 ,  C07C67/00 ,  C07C239/00 ,  C07D201/10 ,  C07D223/10 ,  C07D41/00

    Abstract: 1318618 Omega-lactams SNIA VISCOSA SOC NATIONALE INDUSTRIA APPLICAZIONI VISCOSA SpA 30 June 1970 [5 July 1969] 31572/70 Heading C2C A process for the preparation of an omegalactam having the formula or a precursor thereof (i.e. a compound formed in the process and which can be converted to the lactam by conventional means) comprises nitrosating a cyclomethylene ketene of the formula wherein n has the same value as in the lactam, using a nitrosation agent capable of providing NO + ions in the reaction medium at a temperature of from -60‹ C. to +100‹ C. The nitrosation is preferably carried out in an organic solvent, e.g. CCl 4 or a liquid hydrocarbon using a nitrosating agent of the formula NOX wherein X is nitro, chloro, bisulphate, alkoxy or aryloxy, the molar ratio of the ketene and nitrosating agent (expressed in terms of its content of NO) being between 0À6 : 1 and 1À1 : 1.

    213.
    发明专利
    未知

    公开(公告)号：DE1620569B2

    公开(公告)日：1973-04-19

    申请号：DE1620569

    申请日：1963-05-03

    IPC: C07D201/04 ,  C07D201/10 ,  C07D41/00

    Abstract: Cyclododecanoneoxime is prepared by irradiatcyclododecane in presence of a chlorine-containing nitrosation agent and a cycloalkane (up to C8), separating the resulting oil containing oxime hydrochlorides and diluting with water to precipitate cyclododecanoneoxime. The remaining solution may be neutralized to a pH at least 6.0 with aqueous alkali to precipitate the other oxime. By effecting the Beckmann rearrangement on the said oil a mixture of lactams is obtained which on dilution with water affords o -lauric lactam. In an example, e -caprolactam is recovered from the filtrate. Specification 1,010,151 is referred to.

    214.
    发明专利
    未知

    公开(公告)号：SU368750A3

    公开(公告)日：1973-01-26

    申请号：SU1482612

    申请日：1970-10-01

    IPC: C07D201/10 ,  C07D201/02 ,  C07D41/06

    Abstract: 1297317 #-caprolactam RHONE-POULENC SA 2 Oct 1970 [3 Oct 1969] 47073/70 Heading C2C #-Caprolactam is prepared from a cyclohexane oxidation product containing cyclohexyl hydroperoxide and oxidation by-products including 6- hydroperoxyhexanoic acid which has been obtained by liquid phase oxidation of cyclohexane, without a metal catalyst, using a molecular oxygen containing gas, by washing the oxidation product with water, separating the resulting aqueous phase containing 6- hydroperoxy-hexanoic acid, and heating the 6-hydroperoxy-hexanoic acid under elevated pressure with ammonia and hydrogen in the presence of a hydrogenation catalyst. The oxidation product is suitably washed with 0À01 to 1À0 times its weight of water at 5-100‹ C. and the aqueous phase, prior to being heated with ammonia and hydrogen may be extracted with a liquid hydrocarbon or a water-immiscible solvent comprising an alcohol, ester or ketone; the aqueous phase may then be heated at 200- 300‹ C. under a pressure of 10-200 bars in the presence of hydrogen and 5-25 mols. of ammonia per mol. of 6-hydroperoxy-hexanoic acid. A preferred starting material is a cyclohexane solution of cyclohexyl hydroperoxide in which the oxidized products, which are less volatile than cyclohexane, contain at least 50% by wt. of peroxidic products; suitable hydrogenation catalysts include nickel, platinum, palladium, ruthenium and rhodium which may be supported.

    217.
    发明专利
    未知

    公开(公告)号：DE2048575A1

    公开(公告)日：1971-04-08

    申请号：DE2048575

    申请日：1970-10-02

    IPC: C07D201/10 ,  C07D201/02 ,  C07D41/06

    Abstract: 1297317 #-caprolactam RHONE-POULENC SA 2 Oct 1970 [3 Oct 1969] 47073/70 Heading C2C #-Caprolactam is prepared from a cyclohexane oxidation product containing cyclohexyl hydroperoxide and oxidation by-products including 6- hydroperoxyhexanoic acid which has been obtained by liquid phase oxidation of cyclohexane, without a metal catalyst, using a molecular oxygen containing gas, by washing the oxidation product with water, separating the resulting aqueous phase containing 6- hydroperoxy-hexanoic acid, and heating the 6-hydroperoxy-hexanoic acid under elevated pressure with ammonia and hydrogen in the presence of a hydrogenation catalyst. The oxidation product is suitably washed with 0À01 to 1À0 times its weight of water at 5-100‹ C. and the aqueous phase, prior to being heated with ammonia and hydrogen may be extracted with a liquid hydrocarbon or a water-immiscible solvent comprising an alcohol, ester or ketone; the aqueous phase may then be heated at 200- 300‹ C. under a pressure of 10-200 bars in the presence of hydrogen and 5-25 mols. of ammonia per mol. of 6-hydroperoxy-hexanoic acid. A preferred starting material is a cyclohexane solution of cyclohexyl hydroperoxide in which the oxidized products, which are less volatile than cyclohexane, contain at least 50% by wt. of peroxidic products; suitable hydrogenation catalysts include nickel, platinum, palladium, ruthenium and rhodium which may be supported.

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