公开(公告)号：EP1362842A4

公开(公告)日：2005-06-29

申请号：EP01272302

申请日：2001-12-25

Applicant: TOSOH F TECH INC

Inventor： KONDO NORIHISA ,  MIMURA HIDEYUKI ,  NUKUI KAZUNORI ,  KAWADA KOSUKE ,  ARAI SHOJI

IPC: C07C67/307 ,  C07C67/54 ,  C07C67/58 ,  C07C69/716 ,  C07C69/72 ,  C07C69/738

CPC classification number: C07C67/58 ,  C07C67/307 ,  C07C69/738 ,  C07C69/716

Abstract: 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.

Abstract translation: 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。

公开(公告)号：EP1236706A4

公开(公告)日：2005-02-16

申请号：EP00970026

申请日：2000-10-24

Applicant: TOSOH F TECH INC

Inventor： NUKUI KAZUNORI ,  ABE HIROYUKI ,  NISHIDA TAKUJI ,  ARAI SHOJI

IPC: C01D3/04 ,  C05D1/02 ,  C07C27/00 ,  C07C29/09 ,  C07C29/124 ,  C07C31/38 ,  C07C67/10 ,  C07C29/58 ,  C07C69/62

CPC classification number: C07C29/095 ,  C05D1/02 ,  C07C67/10 ,  C07C69/63 ,  C07C31/38

Abstract: By making use of potassium chloride by-product that is produced in large amounts in a production process of 2,2,2-trifluoroethanol and its esters, potassium chloride suitable for use as a fertilizer is produced. Accordingly, the present invention makes it possible not only to effectively make use of the potassium chloride by-product, but also to reduce the cost in processing the waste products and prevent environmental pollution. The present invention provides a potassium chloride by-product for use as a fertilizer, the potassium chloride by-product produced in a process in which 1,1,1-trifluoro-2-chloroethane is reacted with a potassium salt of an organic carboxylic acid in the presence of polar aprotic solvent to form 2,2,2-trifluoroethanol and/or 2,2,2-trifluoroethyl ester of organic carboxylic acid, the potassium chloride by-product being characterized in that it contains organic materials in an amount of 3wt% or less.

公开(公告)号：EP1426351A4

公开(公告)日：2006-03-01

申请号：EP02760828

申请日：2002-09-13

Applicant: TOSOH F TECH INC

Inventor： NAGASAKI NORITAKA ,  KAWAMURA TSUYOSHI ,  NUKUI KAZUNORI ,  ARAI SHOJI

IPC: C07C29/124 ,  C07C29/80 ,  C07C31/38 ,  C07C51/09 ,  C07C59/01

CPC classification number: C07C29/124 ,  C07C31/38

Abstract: The invention provides a process for the preparation of 2,2,2-trifluoroethanol by reacting a Ϝ-hydroxybutyric acid salt with 1,1,1-trifluoro-2-chloroethane which brings about an increase in the yield of 2,2,2-trifluoroethanol and enables easy separation of by-product salts and recovery and recycling of an aprotic polar solvent. The invention relates to a process for the preparation of 2,2,2-trifluoroethanol by reacting a Ϝ-hydroxybutyric acid salt with 1,1,1-trifluoro-2-chloroethane in an aprotic polar solvent, characterized by using a Ϝ-hydroxybutyric acid salt having a 4,4’-oxydibutyric acid content of 6 wt% or below.

公开(公告)号：EP0891962A4

公开(公告)日：1999-09-01

申请号：EP97907369

申请日：1997-03-18

Applicant: F TECH INC

Inventor： NUKUI KAZUNORI ,  FUKAMI SHINJI ,  KAWADA KOSUKE

IPC: C07D307/33 ,  B01J27/02 ,  B01J27/12 ,  B01J31/02 ,  B01J31/04 ,  C07B39/00 ,  C07B61/00 ,  C07C45/63 ,  C07C47/14 ,  C07C49/167 ,  C07C49/185 ,  C07C49/463 ,  C07C49/80 ,  C07C67/307 ,  C07C69/716 ,  C07C69/738 ,  C07C69/757 ,  C07C205/43 ,  C07C205/45 ,  C07D211/78 ,  C07D211/86 ,  C07D309/32 ,  C07J1/00 ,  C07C49/16 ,  C07C49/227 ,  C07C49/457 ,  C07C49/687

CPC classification number: C07J1/0011 ,  C07B39/00 ,  C07C45/63 ,  C07C67/307 ,  C07C205/43 ,  C07C205/45 ,  C07C69/716 ,  C07C47/14 ,  C07C49/16 ,  C07C49/227 ,  C07C49/457 ,  C07C49/687 ,  C07C49/80 ,  C07C69/738 ,  C07C69/757

Abstract: A process for the preparation of fluorinated dicarbonyl compounds of general formula (2), comprising reacting dicarbonyl compounds of general formula (1) with fluorine gas without any solvent in the presence of one or more acids selected from among trifluoromethanesulfonic acid, methanesulfonic acid, hydrofluoric acid, sulfuric acid, trifluoroacetic acid, boron trifluoride and sulfonated polymers wherein R?1, R2 and R3¿ are each hydrogen, alkyl or the like; and R?1a, R2a and R3a¿ are each the same as defined for R?1, R2 and R3¿, or alternatively when R?1, R2 and R3¿ are each hydrogen, the hydrogen may be replaced by fluorine, while when R?1, R2 and R3¿ are each optionally substituted alkyl, one or more hydrogen atoms on the α-position carbon atom to the CO-group may be replaced by fluorine. This process can give fluorinated dicarbonyl compounds in high yields and at high selectivity.