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    Process For the Preparation of Highly Pure (E) N,N-Diethyl-2-Cyano-3-(3,4-Dihydroxy-5-Nitro Phenyl) Acrylamide (Entacapone)
    1.
    发明申请
    Process For the Preparation of Highly Pure (E) N,N-Diethyl-2-Cyano-3-(3,4-Dihydroxy-5-Nitro Phenyl) Acrylamide (Entacapone) 审中-公开
    制备高纯度（E）N，N-二乙基-2-氰基-3-（3,4-二羟基-5-硝基苯基）丙烯酰胺（恩他卡朋）的方法

    公开(公告)号：US20080319226A1

    公开(公告)日：2008-12-25

    申请号：US12092657

    申请日：2005-11-09

    申请人： Venkatasubramanian Radhakrishnan Tarur ,  Dhananjay Govind Sathe ,  Nandu Baban Bhise ,  Avinash Venkatraman Naidu ,  Umesh Parashram Aher ,  Sachin Shivaji Patil

    发明人： Venkatasubramanian Radhakrishnan Tarur ,  Dhananjay Govind Sathe ,  Nandu Baban Bhise ,  Avinash Venkatraman Naidu ,  Umesh Parashram Aher ,  Sachin Shivaji Patil

    IPC分类号： C07C231/00

    CPC分类号： C07C253/30 ,  C07C253/34 ,  C07C255/41

    摘要： A process for the preparation of highly pure (E)-N,N-diethyl-2-cyano-3-(3,4-dihydroxy-5-nitrophenyl)acrylamide (Entacapone). It comprises condensing 3,4-dihydroxy-5-nitro benzaldehyde with N,N-diethyl cyano acetamide in an organic solvent in the presence of an organic base and an acid under reflux conditions followed by distilling off the solvent under vacuum and treating the residue with a lower aliphatic carboxylic acid at 40-8O0 C. The resulting residue is extracted with a chlorinated solvent and the solvent is distilled off under vacuum. The resulting residue is extracted with an organic solvent to obtain crude N,N-diethyl-2-cyano-3-3,4-dihydroxy-5-nitrophenyl)acrylamide. The crude product N,N-diethyl-2-cyano-3-(3,4-dihydroxy-5-nitrophenyl) acrylamide formed is treated with a mixture of organic alcohol and organic acid in the molar ratio of the crude product to organic alcohol 1:5 to 15 and crude product to organic acid 1:1 to 3 under reflux conditions.

    摘要翻译： 制备高纯度（E）-N，N-二乙基-2-氰基-3-（3,4-二羟基-5-硝基苯基）丙烯酰胺（恩他卡朋）的方法。 它包括在有机碱和酸的存在下，在回流条件下，将3,4-二羟基-5-硝基苯甲醛与N，N-二乙基氰基乙酰胺在有机溶剂中缩合，然后在真空下蒸除溶剂，并处理残余物 与40-80℃的低级脂族羧酸反应。所得残余物用氯化溶剂萃取，真空蒸除溶剂。 所得残余物用有机溶剂萃取，得到粗N，N-二乙基-2-氰基-3-3,4-二羟基-5-硝基苯基）丙烯酰胺。 所形成的粗产物N，N-二乙基-2-氰基-3-（3,4-二羟基-5-硝基苯基）丙烯酰胺以有机醇与有机酸的混合物以粗产物与有机醇的摩尔比 1:5至15，并在回流条件下将粗产物与有机酸1:1至3反应。