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    METHOD FOR PREPARING PREGABALIN INTERMEDIATE, 3-CARBAMOYMETHYL-5-METHYLHEXANOIC ACID, USING SOLVENT-FREE REACTION
    3.
    发明公开
    METHOD FOR PREPARING PREGABALIN INTERMEDIATE, 3-CARBAMOYMETHYL-5-METHYLHEXANOIC ACID, USING SOLVENT-FREE REACTION 审中-公开
    用无溶剂反应制备孕烷中间体3-氨基甲酰基甲基-5-甲基己二酸的方法

    公开(公告)号：EP3275860A1

    公开(公告)日：2018-01-31

    申请号：EP16771321.3

    申请日：2016-03-25

    申请人： Zhejiang Huahai Pharmaceutical Co., Ltd

    发明人： LIU, Musong ,  ZHANG, Wenling ,  WANG, Peng

    IPC分类号： C07C233/05 ,  C07C231/02

    CPC分类号： C07C231/02 ,  C07C231/24 ,  C07C233/05

    摘要： The present invention provides a method for preparing a pregabalin intermediate3-carbamoymethyl-5-methylhexanoic acid without solvent. The method comprises the following steps: a) cooling an ammonia water system to a certain temperature; b) adding 3-isobutylglutaric anhydride dropwise to the system, then keeping temperature, and reacting; c) after completing the reaction, adding an acid to the system to adjust PH; d) after adjusting PH, cooling, then keeping temperature, crystallizing, then suction filtering and drying; and e) adding a solvent to the dried substance, slurrying, and suction filtering and drying to obtain the final product. The method provided in the present invention for preparing 3-carbamoymethyl-5-methylhexanoic acid is high-yield, green, environmentally-friendly, simple and convenient, and of less pollution.

    摘要翻译： 本发明提供了一种无溶剂制备普瑞巴林中间体3-氨基甲酰基甲基-5-甲基己酸的方法。 该方法包括以下步骤：a）将氨水系统冷却至一定温度; b）向体系中滴加3-异丁基戊二酸酐，然后保持温度并反应; c）完成反应后，向体系中加入酸调节PH; d）调整PH值后，冷却，然后保温，结晶，然后抽滤，干燥。 和e）向干燥的物质中加入溶剂，浆化和吸滤和干燥以获得最终产物。 本发明提供的制备3-氨基甲酰甲基-5-甲基己酸的方法收率高，绿色环保，简单方便，污染少。

    KONTINUIERLICHES VERFAHREN ZUR ABTRENNUNG VON SALZEN BEI DER HERSTELLUNG VON DIMETHYLACETAMID
    7.
    发明公开
    KONTINUIERLICHES VERFAHREN ZUR ABTRENNUNG VON SALZEN BEI DER HERSTELLUNG VON DIMETHYLACETAMID 审中-公开
    连续法盐的二甲基乙酰胺制造分离

    公开(公告)号：EP2935203A1

    公开(公告)日：2015-10-28

    申请号：EP13815464.6

    申请日：2013-12-18

    申请人： BASF SE

    发明人： LANG, Ortmund ,  ASPRION, Norbert ,  BINDER, Axel ,  METZEN, Bernd ,  WIGBERS, Christof Wilhelm ,  KUBANEK, Petr ,  STEINHILBER, Thomas

    IPC分类号： C07C231/02

    CPC分类号： C07C231/24 ,  B01D3/06 ,  B01D3/42 ,  C07C231/02 ,  C07C233/05

    摘要： The invention relates to a continuous method for separating out a solid, saline phase containing alkaline and/or alkaline earth acetates from the product mixture of the production of N,N-dimethylacetamide (DMAc) by reacting methyl acetate (MeOAc) with dimethylamine (DMA) in the presence of a catalyst containing N,N-dimethylacetamide (DMAc), methyl acetate (MeOAc), dimethylamine (DMA) and a catalyst, with the following method steps: level-regulated feeding of the product mix as a feed flow into an evaporation container of a forced circulation reboiler; flash evaporation of volatile components of the product mix in the forced circulation reboiler with the formation of a vapour phase containing N,N-dimethylacetamide (DMAc) and precipitation of a solid, saline phase containing alkaline or alkaline earth acetates; feed back of the volatile components of the product mixture obtained after flash evaporation; discharging an N,N-dimethylacetamide (DMAC) containing a vapour phase from the evaporator container as a discharge flow; concentration of the solid, saline phase containing alkaline or alkaline earth acetates in the forced circulation reboiling circuit of the forced circulation reboiler; separation of a partial flow comprising the solid, saline phase containing alkaline and/or alkaline earth acetates from the forced circulation reboiling circuit of the forced circulation reboiler; solid/liquid separation of the separated partial flow in at least one separator into a solid, saline phase containing alkaline and/or alkaline earth acetates and a liquid phase; and feeding of the liquid phase obtained after the solid/liquid separation back into the forced circulation reboiling circuit as a feedback flow. The method is characterized in that the volatile components of the product mix obtained after flash evaporation and the solid, saline phase containing alkaline and/or alkaline earth acetates are fed back into the evaporation container through an infeed which ends in a range from 30 cm above the level surface to 20 cm below the level surface of the fill level of the evaporation container.