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1. 发明授权

EP1426351B1 PROCESS FOR PREPARATION OF 2,2,2-TRIFLUOROETHANOL 有权
标题翻译：用于生产2,2,2-三氟乙醇
公开(公告)号：EP1426351B1
公开(公告)日：2013-06-19
申请号：EP02760828.0
申请日：2002-09-13
申请人： Tosoh F-Tech, Inc.
发明人： NAGASAKI, Noritaka , KAWAMURA, Tsuyoshi , NUKUI, Kazunori , ARAI, Shoji
IPC分类号： C07C29/124 , C07C29/80 , C07C31/38 , C07C51/09 , C07C59/01
CPC分类号： C07C29/124 , C07C31/38

2. 发明授权

EP1362842B1 PROCESS FOR PRODUCING 2-FLUORO-3-OXOALKYLCARBOXYLIC ACID ESTER 有权
标题翻译：生产2-氟-3-氧代烷基羧酸酯的方法
公开(公告)号：EP1362842B1
公开(公告)日：2007-03-14
申请号：EP01272302.9
申请日：2001-12-25
申请人： Tosoh F-Tech, Inc.
发明人： KONDO, Norihisa , MIMURA, Hideyuki , NUKUI, Kazunori , KAWADA, Kosuke , ARAI, Shoji
IPC分类号： C07C67/307 , C07C67/54 , C07C67/58 , C07C69/72 , C07C69/716 , C07C69/738
CPC分类号： C07C67/58 , C07C67/307 , C07C69/738 , C07C69/716
摘要： A process for preparing 2-fluoro-3-oxoalkylcarboxylic acid esters by fluorinating a 3-oxoalkylcarboxylic acid ester with fluorine gas, characterized in that the concentration of the 3-oxoalkylcarboxylic acid ester in the reaction fluid is kept at 3 wt% or above; and a process for purifying 2-fluoro-3- oxoalkylcarboxylic acid esters, characterized by washing a product of fluorination of a 3-oxoalkylcarboxylic acid ester with at least thrice as much water as the substrate to thereby obtain a purified 2-fluoro-3-oxoalkylcarboxylic acid ester in a high yield. According to these processes, high-purity 2-fluoro-3-oxoalkylcarboxylic acid esters useful as intermediates for drugs or agricultural chemicals can be efficiently prepared through inhibition of by-product formation or efficient purification of products of fluorination of 3-oxoalkylcarboxylic acid esters.
摘要翻译：其特征在于，反应液中的3-氧代烷基羧酸酯的浓度保持在3重量％以上，其特征在于，所述反应液中的3-氧代烷基羧酸酯的浓度为3重量％以上。和纯化2-氟-3-氧代烷基羧酸酯的方法，其特征在于用至少为底物3倍的水洗涤3-氧代烷基羧酸酯的氟化产物，从而得到纯化的2-氟-3- 氧代烷基羧酸酯。根据这些方法，通过抑制副产物形成或有效纯化3-氧代烷基羧酸酯的氟化产物，可以有效地制备用作药物或农药中间体的高纯度2-氟-3-氧代烷基羧酸酯。

3. 发明公开

EP1426351A1 PROCESS FOR PREPARATION OF 2,2,2-TRIFLUOROETHANOL 有权
标题翻译： VERFAHREN ZUR HERSTELLUNG VON 2,2,2-TRIFLUORETHANOL
公开(公告)号：EP1426351A1
公开(公告)日：2004-06-09
申请号：EP02760828.0
申请日：2002-09-13
申请人： Tosoh F-Tech, Inc.
发明人： NAGASAKI, Noritaka , KAWAMURA, Tsuyoshi , NUKUI, Kazunori , ARAI, Shoji
IPC分类号： C07C29/124 , C07C29/80 , C07C31/38 , C07C51/09 , C07C59/01
CPC分类号： C07C29/124 , C07C31/38
摘要： A method for producing 2,2,2-trifluoroethanol in which a γ-hydroxybutyric acid salt is reacted with 1,1,1-trifluoro-2-chloroethane to generate 2,2,2-trifluoroethanol is provided. This method leads to increased yields of 2,2,2-trifluoroethanol, facilitates the separation of salt byproducts and allows the recycling of an aprotic polar solvent.
The present invention concerns a method for producing 2,2,2-trifluoroethanol in which a γ-hydroxybutyric acid salt is reacted with 1,1,1-trifluoro-2-chloroethane in an aprotic polar solvent to generate 2,2,2-trifluoroethanol. This method is characterized in that the γ-hydroxybutyric acid salt used contains no more than 6wt% of 4,4'-oxybis(butyric acid).
摘要翻译：提供一种制备2,2,2-三氟乙醇的方法，其中将γ-羟基丁酸盐与1,1,1-三氟-2-氯乙烷反应生成2,2,2-三氟乙醇。该方法导致2,2,2-三氟乙醇的产率增加，促进了盐副产物的分离并允许非质子极性溶剂的再循环。本发明涉及一种制备2,2,2-三氟乙醇的方法，其中γ-羟基丁酸盐在非质子极性溶剂中与1,1,1-三氟-2-氯乙烷反应生成2， 2,2-三氟乙醇。该方法的特征在于所用的γ-羟基丁酸盐含有不超过6重量％的4,4'-氧双（丁酸）。

4. 发明公开

EP1362842A1 PROCESS FOR PRODUCING 2-FLUORO-3-OXOALKYLCARBOXYLIC ACID ESTER 有权
标题翻译：生产2-氟-3-氧代烷基羧酸酯的方法
公开(公告)号：EP1362842A1
公开(公告)日：2003-11-19
申请号：EP01272302.9
申请日：2001-12-25
申请人： Tosoh F-Tech, Inc.
发明人： KONDO, Norihisa , MIMURA, Hideyuki , NUKUI, Kazunori , KAWADA, Kosuke , ARAI, Shoji
IPC分类号： C07C67/307 , C07C67/54 , C07C67/58 , C07C69/72 , C07C69/716 , C07C69/738
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 3wt% 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：提供了通过用氟气对3-氧代烷基羧酸酯进行氟化来制备2-氟-3-氧代烷基羧酸酯的方法。该方法的特征在于，氟化反应混合物中3-氧代烷基羧酸酯的浓度保持在3wt％或更高。本发明还提供了一种纯化2-氟-3-氧代烷基羧酸酯的方法，其特征在于通过洗涤氟化3-氧代烷基羧酸酯3次或更多次而以高收率和低杂质生产2-氟-3-氧代烷基羧酸酯尽可能多的水作为反应混合物的量。根据本发明的方法，不仅可以使不需要的副产物的产生最小化，而且可以以有效的方式纯化氟化3-氧代烷基羧酸酯。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，这是一种用于生产各种医药和农药的有用中间体材料。

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