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    • 1. 发明授权
    • Process for producing fluoro-compounds
    • 氟化合物的制备方法
    • US07615669B2
    • 2009-11-10
    • US11887135
    • 2006-03-22
    • Norihisa KondoAkio WatanabeHiroki KanezakiKosuke Kawada
    • Norihisa KondoAkio WatanabeHiroki KanezakiKosuke Kawada
    • C07C31/34C07C31/38
    • C07C67/307C07B39/00C07C17/16C07C2601/08C07C2603/74C07C19/08C07C23/38C07C23/08C07C69/65C07C69/63
    • 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.
    • 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。
    • 2. 发明申请
    • Process for producing fluoro-compounds
    • 氟化合物的制备方法
    • US20090030228A1
    • 2009-01-29
    • US11887135
    • 2006-03-22
    • Norihisa KondoAkio WatanabeHiroki KanezakiKosuke Kawada
    • Norihisa KondoAkio WatanabeHiroki KanezakiKosuke Kawada
    • C07C69/76C07C19/08
    • C07C67/307C07B39/00C07C17/16C07C2601/08C07C2603/74C07C19/08C07C23/38C07C23/08C07C69/65C07C69/63
    • 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.
    • 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。
    • 3. 发明授权
    • Process for preparing 2-fluoro-3-oxoalkylcarboxylic acid ester
    • 2-氟-3-氧代烷基羧酸酯的制备方法
    • US07019162B2
    • 2006-03-28
    • US10451814
    • 2001-12-25
    • Norihisa KondoHideyuki MimuraKazunori NukuiKosuke KawadaShoji Arai
    • Norihisa KondoHideyuki MimuraKazunori NukuiKosuke KawadaShoji Arai
    • C07C69/66
    • C07C67/58C07C67/307C07C69/738C07C69/716
    • 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.
    • 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。