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    Process for the manufacture of methyl limonitrile
    15.
    发明授权
    Process for the manufacture of methyl limonitrile 有权
    制备甲基有限公司的方法

    公开(公告)号：US09458096B2

    公开(公告)日：2016-10-04

    申请号：US14377095

    申请日：2013-02-11

    Applicant: DSM IP ASSETS B.V.

    Inventor： Angela Wildermann ,  Werner Bonrath ,  Raphael Beumer ,  Silke Dorn

    IPC: C07C253/30 ,  C07C255/07 ,  C11D3/50 ,  C07C253/10 ,  C07C253/34

    CPC classification number: C07C253/10 ,  C07C253/30 ,  C07C253/34 ,  C07C255/07

    Abstract: The present invention is directed to a process for the manufacture of methyl limonitrile comprising a mixture of 3,7-dimethyl-2,6-nonadiene nitrile, 3,7-dimethyl-3,6-nonadiene nitrile and 7-methyl-3-methylene-6-nonene nitrile comprising the following steps: a) reacting 6-methyl-5-octen-2-one with cyano acetic acid and removing carbon dioxide and water, wherein the reaction and the removal of carbon dioxide and water are performed in the presence of a base and a co-base 1 in an organic solvent, and wherein the organic solvent is a solvent which forms a heteroazeotrop with water; b) removing the solvent and the base of the reaction mixture obtained after having performed step a) or step c) by distillation to obtain a reaction mixture, whereby this step may optionally be performed in the presence of a co-base 2; c) isomerizing the reaction mixture obtained after having performed step a) or step b) to obtain an isomerized reaction mixture in the presence of a co-base 2; whereby step b) can be performed before or after step c).

    Abstract translation: 本发明涉及一种制备甲基有限公司的方法，该方法包括3,7-二甲基-2,6-壬二烯腈，3,7-二甲基-3,6-壬二烯腈和7-甲基-3- 亚甲基-6-壬烯腈包括以下步骤：a）使6-甲基-5-辛烯-2-酮与氰基乙酸反应并除去二氧化碳和水，其中二氧化碳和水的反应和除去在 在有机溶剂中存在碱和共碱1，其中有机溶剂是与水形成杂合性的溶剂; b）通过蒸馏除去在进行步骤a）或步骤c）之后获得的反应混合物的溶剂和碱，得到反应混合物，由此该步骤可任选地在共碱2存在下进行; c）使在步骤a）或步骤b）中获得的反应混合物异构化，以在共碱2存在下得到异构化反应混合物; 由此步骤b）可以在步骤c）之前或之后进行。

    Process for the manufacture of methyl limonitrile
    19.
    发明授权
    Process for the manufacture of methyl limonitrile 有权
    制备甲基有限公司的方法

    公开(公告)号：US09340750B2

    公开(公告)日：2016-05-17

    申请号：US14378551

    申请日：2013-02-11

    Applicant: DSM IP ASSETS B.V.

    Inventor： Raphael Beumer ,  Werner Bonrath ,  Silke Dorn ,  Angela Wildermann

    IPC: C11B9/00 ,  C07C253/30

    CPC classification number: C11B9/0023 ,  C07C253/30 ,  C07C255/07

    Abstract: The present invention is directed to a process for the manufacture of methyl limonitrile comprising a mixture of 3,7-dimethyl-2,6-nonadiene nitrile, 3,7-dimethyl-3,6-nonadiene nitrile and 7-methyl-3-methylene-6-nonene nitrile comprising the following steps: a) reacting 6-methyl-5-octen-2-one with cyano acetic acid and removing carbon dioxide and water, wherein the reaction and the removal of carbon dioxide and water are performed in the presence of a base and a co-base in an organic solvent, wherein the base is pyridine, wherein the co-base is 1,4-diamino butane, and wherein the organic solvent is a solvent which forms a heteroazeotrop with water; b) removing the solvent and pyridine of the reaction mixture obtained after having performed step a) or step c) by distillation to obtain a reaction mixture; c) isomerizing the reaction mixture obtained after having performed step a) or step b) to obtain an isomerized reaction mixture; whereby step b) can be performed before or after step c).

    Abstract translation: 本发明涉及一种制备甲基有限公司的方法，该方法包括3,7-二甲基-2,6-壬二烯腈，3,7-二甲基-3,6-壬二烯腈和7-甲基-3- 亚甲基-6-壬烯腈包括以下步骤：a）使6-甲基-5-辛烯-2-酮与氰基乙酸反应并除去二氧化碳和水，其中二氧化碳和水的反应和除去在 在有机溶剂中存在碱和共碱，其中所述碱为吡啶，其中所述共碱为1,4-二氨基丁烷，并且其中所述有机溶剂是与水形成杂合性的溶剂; b）在通过蒸馏进行步骤a）或步骤c）之后，除去反应混合物中的溶剂和吡啶，得到反应混合物; c）使进行步骤a）或步骤b）后得到的反应混合物异构化得到异构化反应混合物; 由此步骤b）可以在步骤c）之前或之后进行。

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