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    Process for preparing 2-fluoro-3-oxoalkylcarboxylic acid ester
    1.
    发明授权
    Process for preparing 2-fluoro-3-oxoalkylcarboxylic acid ester 失效
    2-氟-3-氧代烷基羧酸酯的制备方法

    公开(公告)号：US07019162B2

    公开(公告)日：2006-03-28

    申请号：US10451814

    申请日：2001-12-25

    申请人： Norihisa Kondo ,  Hideyuki Mimura ,  Kazunori Nukui ,  Kosuke Kawada ,  Shoji Arai

    发明人： Norihisa Kondo ,  Hideyuki Mimura ,  Kazunori Nukui ,  Kosuke Kawada ,  Shoji Arai

    IPC分类号： C07C69/66

    CPC分类号： C07C67/58 ,  C07C67/307 ,  C07C69/738 ,  C07C69/716

    摘要： A process for producing a 2-fluoro-3-oxoalkylcarboxylic acid ester by fluorinating 3-oxoalkylcarboxylic acid ester with a fluorine gas is provided. The process is characterized in that the concentration of 3-oxoalkylcarboxylic acid ester in the reaction mixture for fluorination is maintained at 3 wt % or higher. Also provided is a process for purifying 2-fluoro-3-oxoalkylcarboxylic acid ester characterized in that 2-fluoro-3-oxoalkylcarboxylic acid ester is produced at high yield and with less impurities by washing fluorinated 3-oxoalkylcarboxylic acid ester with 3 or more times as much water as the amount of reaction mixture. According to the processes of the present invention, not only is the generation of unwanted by-products minimized, but fluorinated 3-oxoalkylcarboxylic acid ester can be purified in an efficient manner. Thus, the present invention permits efficient production of considerably pure 2-fluoro-3-oxoalkylcarboxylic acid ester, a useful intermediate material in the production of various medical and agricultural agents.

    摘要翻译： 提供了通过用氟气氟化3-氧代烷基羧酸酯来制备2-氟-3-氧代烷基羧酸酯的方法。 该方法的特征在于用于氟化的反应混合物中3-氧代烷基羧酸酯的浓度保持在3重量％以上。 还提供了一种纯化2-氟-3-氧代烷基羧酸酯的方法，其特征在于2-氟-3-氧代烷基羧酸酯以高产率制备，通过用氟化3-氧代烷基羧酸酯洗涤3次或更多次而得到较少的杂质 与反应混合物的量一样多的水。 根据本发明的方法，不仅产生不想要的副产物最小化，而且氟化的3-氧代烷基羧酸酯可以以有效的方式被纯化。 因此，本发明允许有效地生产相当纯的2-氟-3-氧代烷基羧酸酯，这是生产各种医药和农药的有用的中间体材料。

    Process for producing fluorinated alcohol
    2.
    发明授权
    Process for producing fluorinated alcohol 失效
    制备氟化醇的方法

    公开(公告)号：US06894197B2

    公开(公告)日：2005-05-17

    申请号：US10476540

    申请日：2002-07-01

    申请人： Hideyuki Mimura ,  Kosuke Kawada ,  Shoji Arai

    发明人： Hideyuki Mimura ,  Kosuke Kawada ,  Shoji Arai

    IPC分类号： C07C29/124 ,  C07C31/38 ,  C07C31/42 ,  C07C31/44 ,  C07C205/43 ,  C07C233/10 ,  C07C233/28 ,  C07C233/33 ,  C07C233/44 ,  C07C233/55 ,  C07F9/12 ,  C07C31/34

    CPC分类号： C07C29/124 ,  C07C31/38

    摘要： A method for producing fluorinated alcohols from fluorinated alkyl halides can produce fluorinated alcohols at high product yield and at high selectivity in a single-step reaction. The method eliminates the need to use heavy metals and other toxic compounds that are difficult to handle or process.Specifically, the method produces a fluorinated alcohol represented by the following general formula (2): Rf(A)OH  (2) wherein Rf represents a perfluoroalkyl group having 1 to 10 carbon atoms; and A represents a straight-chained or branched saturated hydrocarbon group having 3 to 10 carbon atoms. The method is characterized in that it allows a fluorinated alkyl halide represented by the following general formula (1) to react with an alkali metal salt of 4-hydroxybutyrate in a gamma-butyrolactone solvent: Rf(A)X  (1) wherein Rf and A are as defined above; and X represents a halogen atom.

    摘要翻译： 从氟化烷基卤化物制备氟化醇的方法可以以高产率和在一步反应中以高选择性产生氟化醇。 该方法无需使用难处理或加工的重金属和其他有毒化合物。 具体地说，该方法产生由以下通式（2）表示的氟化醇：<？in-line-formula description =“In-line formula”end =“lead”？> Rf（A）OH（2） 在线公式描述=“In-line Formula”end =“tail”？>其中Rf表示具有1-10个碳原子的全氟烷基; A表示碳原子数3〜10的直链状或支链状的饱和烃基。 该方法的特征在于，其允许由以下通式（1）表示的氟化烷基卤在γ-丁内酯溶剂中与4-羟基丁酸的碱金属盐反应：<？在线配方说明=“In 线型公式“end =”lead“？> Rf（A）X（1）<？in-line-formula description =”In-line Formulas“end =”tail“？>其中Rf和A如上所定义; X表示卤素原子。

    Method of purifying and separating 2-fluoro-3-oxoalkylcarboxylic acid ester
    3.
    发明授权
    Method of purifying and separating 2-fluoro-3-oxoalkylcarboxylic acid ester 失效
    纯化和分离2-氟-3-氧代烷基羧酸酯的方法

    公开(公告)号：US07220878B2

    公开(公告)日：2007-05-22

    申请号：US10490432

    申请日：2001-09-27

    申请人： Norihisa Kondo ,  Hideyuki Mimura ,  Kosuke Kawada ,  Shoji Arai

    发明人： Norihisa Kondo ,  Hideyuki Mimura ,  Kosuke Kawada ,  Shoji Arai

    IPC分类号： C07C69/66

    CPC分类号： C07C67/54 ,  C07C69/716

    摘要： The present invention concerns a method for purifying/separating a 2-fluoro-3-oxoalkylcarboxylic acid ester from a reaction mixture resulting from the fluorination of a 3-oxoalkylcarboxylic acid ester. The method involves depleting the reaction mixture of a hydrogen fluoride byproduct; and subsequently, separating the 2-fluoro-3-oxoalkylcarboxylic acid ester by distillation. The 2-fluoro-3-oxoalkylcarboxylic acid ester obtained by the method of the invention is highly pure and is thus suitable for use as an intermediate for the production of pharmacological products or agricultural chemicals.

    摘要翻译： 本发明涉及从3-氧代烷基羧酸酯氟化得到的反应混合物中纯化/分离2-氟-3-氧代烷基羧酸酯的方法。 该方法涉及耗尽氟化氢副产物的反应混合物; 随后通过蒸馏分离2-氟-3-氧代烷基羧酸酯。 通过本发明方法获得的2-氟-3-氧代烷基羧酸酯是高纯度的，因此适合用作生产药物产品或农药的中间体。

    Alpha-pentafluoroethylacrylic acid derivative and process for producing the same
    4.
    发明申请
    Alpha-pentafluoroethylacrylic acid derivative and process for producing the same 审中-公开
    α-五氟乙基丙烯酸衍生物及其制备方法

    公开(公告)号：US20060183937A1

    公开(公告)日：2006-08-17

    申请号：US10550066

    申请日：2004-03-24

    申请人： Kenji Tokuhisa ,  Hideyuki Mimura ,  Kosuke Kawada ,  Shoji Arai

    发明人： Kenji Tokuhisa ,  Hideyuki Mimura ,  Kosuke Kawada ,  Shoji Arai

    IPC分类号： C07C69/62

    CPC分类号： C07C57/54 ,  C07C57/52

    摘要： An α-pentafluoroethyl acrylic acid derivative represented by the general formula [I]: [wherein R represents a hydrogen atom, a non-substituted or substituted aromatic ring, or a straight or branched alkyl group having 1 to 20 carbon(s) which may have a cyclic moiety optionally substituted with at least one substituent (halogen atom, hydroxyl group, straight or branched alkoxy group having 1 to 10 carbon(s) which may have a cyclic moiety, non-substituted or substituted aromatic group)].

    摘要翻译： 由通式[I]表示的α-五氟乙基丙烯酸衍生物：[其中R表示氢原子，未取代或取代的芳环，或具有1至20个碳的直链或支链烷基，其可以 具有任选被至少一个取代基（卤素原子，羟基，具有1至10个碳原子的直链或支链烷氧基，可以具有环状部分，未取代或取代的芳族基团）取代的环状部分]。

    Process for producing fluoro-compounds
    7.
    发明授权
    Process for producing fluoro-compounds 有权
    氟化合物的制备方法

    公开(公告)号：US07615669B2

    公开(公告)日：2009-11-10

    申请号：US11887135

    申请日：2006-03-22

    申请人： Norihisa Kondo ,  Akio Watanabe ,  Hiroki Kanezaki ,  Kosuke Kawada

    发明人： Norihisa Kondo ,  Akio Watanabe ,  Hiroki Kanezaki ,  Kosuke Kawada

    IPC分类号： C07C31/34 ,  C07C31/38

    CPC分类号： C07C67/307 ,  C07B39/00 ,  C07C17/16 ,  C07C2601/08 ,  C07C2603/74 ,  C07C19/08 ,  C07C23/38 ,  C07C23/08 ,  C07C69/65 ,  C07C69/63

    摘要： The present invention provides a process for producing highly pure fluoro-compounds by making use of N-(2-chloro-1,1,2-trifluoroethyl)diethylamine. The process produces little or no chlorinated by-products. The present invention provides a process for producing a fluoro-compound, comprising fluorinating an alcohol derivative represented by the following general formula (I): R1R2R3COH (I), (wherein R1 represents a hydrogen atom, a substituted or unsubstituted alkyl group, aryl group, alkylcarbonyl group, alkoxycarbonyl group, arylcarbonyl group or aryloxycarbonyl group; and R2 and R3 are each independently a substituted or unsubstituted alkyl group, aryl group, alkylcarbonyl group, alkoxycarbonyl group, arylcarbonyl group or aryloxycarbonyl group, wherein at least two of R1, R2 and R3 may together form part of a ring structure, either with or without a heteroatom) with N,N-diethyl-2-chloro-1,1,2-trifluoroethylamine to form a fluoro-compound represented by the following general formula (2): R1R2R3CF (2), (wherein R1, R2 and R3 are as defined above), the process being characterized in that an alcohol derivative represented by the following general formula (3): R4OH (3), (wherein R4 represents a substituted or unsubstituted alkyl group or aryl group) is added to the reaction system.

    摘要翻译： 本发明提供通过使用N-（2-氯-1,1,2-三氟乙基）二乙胺生产高纯度氟化合物的方法。 该方法几乎不产生或不产生氯化副产物。 本发明提供一种氟化合物的制造方法，其包括将下述通式（I）表示的醇衍生物氟化：R1R2R3COH（I），（其中R1表示氢原子，取代或未取代的烷基，芳基 烷基羰基，烷氧基羰基，芳基羰基或芳氧基羰基; R2和R3各自独立地为取代或未取代的烷基，芳基，烷基羰基，烷氧基羰基，芳基羰基或芳氧基羰基，其中R1，R2中的至少两个 和R3可以一起形成具有或不具有杂原子的环结构的一部分）与N，N-二乙基-2-氯-1,1,2-三氟乙胺反应，形成由以下通式（2）表示的氟化合物 ）：R1R2R3CF（2）（其中R1，R2和R3如上定义），其特征在于由以下通式（3）表示的醇衍生物：R4OH（3），（其中R4表示 是取代或未取代的烷基或芳基）加入到反应体系中。

    Process for producing fluoro-compounds
    8.
    发明申请
    Process for producing fluoro-compounds 有权
    氟化合物的制备方法

    公开(公告)号：US20090030228A1

    公开(公告)日：2009-01-29

    申请号：US11887135

    申请日：2006-03-22

    申请人： Norihisa Kondo ,  Akio Watanabe ,  Hiroki Kanezaki ,  Kosuke Kawada

    发明人： Norihisa Kondo ,  Akio Watanabe ,  Hiroki Kanezaki ,  Kosuke Kawada

    IPC分类号： C07C69/76 ,  C07C19/08

    CPC分类号： C07C67/307 ,  C07B39/00 ,  C07C17/16 ,  C07C2601/08 ,  C07C2603/74 ,  C07C19/08 ,  C07C23/38 ,  C07C23/08 ,  C07C69/65 ,  C07C69/63

    摘要： The present invention provides a process for producing highly pure fluoro-compounds by making use of less costly and readily handleable N-(2-chloro-1,1,2-trifluoroethyl)diethylamine. The process produces little or no chlorinated by-products.Specifically the present invention provides a process for producing a fluoro-compound, comprising fluorinating an alcohol derivative represented by the following general formula (1): R1R2R3COH  (1) (wherein R1 represents a hydrogen atom, a substituted or unsubstituted alkyl group, aryl group, alkylcarbonyl group, alkoxycarbonyl group, arylcarbonyl group or aryloxycarbonyl group; and R2 and R3are each independently a substituted or unsubstituted alkyl group, aryl group, alkylcarbonyl group, alkoxycarbonyl group, arylcarbonyl group or aryloxycarbonyl group, wherein at least two of R1, R2 and R3 may together form part of a ring structure, either with or without a heteroatom) with N,N-diethyl-2-chloro-1,1,2-trifluoroethylamine to form a fluoro-compound represented by the following general formula (2): R1R2R3CF  (2) (wherein R1, R2 and R3 are as defined above), the process being characterized in that an alcohol derivative represented by the following general formula (3): R4OH  (3) (wherein R4 represents a substituted or unsubstituted alkyl group or aryl group) is added to the reaction system.

    摘要翻译： 本发明提供了通过使用成本较低且易于处理的N-（2-氯-1,1,2-三氟乙基）二乙胺制备高纯度氟化合物的方法。 该方法几乎不产生或不产生氯化副产物。 具体地说，本发明提供一种氟化合物的制造方法，其特征在于，含氟化下述通式（1）表示的醇衍生物：＆lt;线内式记载=“在线式”末端=“铅” > R1R2R3COH（1）<？in-line-formula description =“In-line Formulas”end =“tail”？>（其中R1表示氢原子，取代或未取代的烷基，芳基，烷基羰基，烷氧基羰基 ，芳基羰基或芳氧基羰基; R2和R3各自独立地为取代或未取代的烷基，芳基，烷基羰基，烷氧基羰基，芳基羰基或芳氧基羰基，其中R1，R2和R3中的至少两个可以一起形成 具有或不具有杂原子的环结构）与N，N-二乙基-2-氯-1,1,2-三氟乙胺反应以形成由以下通式（2）表示的氟化合物： -formulae description =“在线公式”end =“lead”？> R1R2R3 CF（2）<？in-line-formula description =“In-line Formulas”end =“tail”？>（其中R1，R2和R3如上定义），该方法的特征在于，以 以下通式（3）：<？in-line-formula description =“In-line Formulas”end =“lead”？> R4OH（3）<？in-line-formula description =“In-line Formulas”end =“尾”→（其中R 4表示取代或未取代的烷基或芳基）加入到反应体系中。