公开(公告)号：US20180050976A1

公开(公告)日：2018-02-22

申请号：US15551160

申请日：2016-01-22

申请人： Central Glass Company, Limited

发明人： Shoko ISHII ,  Takako YAMAZAKI ,  Takashi KASHIWABA ,  Ryuichi OKAMOTO ,  Akihiro ISHII

IPC分类号： C07C67/313 ,  C07C67/31

CPC分类号： C07C67/313 ,  C07C67/31 ,  C07C69/716 ,  C07C69/67 ,  C07C69/675

摘要： It is possible to produce a fluorine-containing α-ketocarboxylic ester hydrate by reacting a fluorine-containing α-hydroxycarboxylic ester with sodium hypochlorite or calcium hypochlorite of 21 mass % or greater in mass percentage of composition. Furthermore, it is possible to produce a fluorine-containing α-ketocarboxylic ester by reacting the hydrate with a dehydrating agent. Furthermore, it is possible to produce a fluorine-containing α-ketocarboxylic ester hemiketal by reacting the fluorine-containing α-ketocarboxylic ester hydrate with a lower alcohol or a trialkyl orthocarboxylate. Moreover, it is possible to produce a fluorine-containing α-ketocarboxylic ester by reacting the hemiketal with a dealcoholization agent.

公开(公告)号：US20190389831A1

公开(公告)日：2019-12-26

申请号：US16562214

申请日：2019-09-05

申请人： Central Glass Company, Limited

发明人： Takashi KASHIWABA ,  Takako YAMAZAKI ,  Shoko ISHII ,  Shunsuke MIMURA ,  Masanori FUSHIMI ,  Ryuichi OKAMOTO ,  Haruki KOBAYASHI ,  Manabu YASUMOTO

IPC分类号： C07D327/10 ,  C07C211/27 ,  C07C67/08 ,  C07C69/74 ,  C07C67/52 ,  C07C67/343

摘要： The present invention provides an industrially applicable method for production of a fluorine-containing cyclopropane carboxylic acid compound useful as an intermediate for pharmaceutical and agrichemical products. A fluorine-containing cyclopropane monoester is obtained by: forming a fluorine-containing cyclic sulfate with the use of a fluorine-containing diol compound and sulfuryl fluoride (as a cyclic sulfuric esterification step); reacting the fluorine-containing cyclic sulfate with a malonic diester, thereby forming a fluorine-containing cyclopropane diester (as a cyclopropanation step); and hydrolyzing the fluorine-containing cyclopropane diester (as a hydrolysis step). The fluorine-containing cyclopropane carboxylic acid compound, such as fluorine-containing cyclopropane monoester or its salt, can be obtained with high chemical and optical purity by mixing the fluorine-containing cyclopropane monoester with an amine and subjecting the resulting salt of the fluorine-containing cyclopropane monoester and amine to recrystallization purification.

公开(公告)号：US20180186763A1

公开(公告)日：2018-07-05

申请号：US15741020

申请日：2016-06-24

申请人： CENTRAL GLASS COMPANY, LIMITED

发明人： Takashi KASHIWABA ,  Takako YAMAZAKI ,  Shoko ISHII ,  Shunsuke MIMURA ,  Masanori FUSHIMI ,  Ryuichi OKAMOTO ,  Haruki KOBAYASHI ,  Manabu YASUMOTO

IPC分类号： C07D327/10 ,  C07C67/343 ,  C07C67/52 ,  C07C69/74 ,  C07C211/27 ,  C07C67/08

CPC分类号： C07D327/10 ,  C07B57/00 ,  C07C67/08 ,  C07C67/313 ,  C07C67/343 ,  C07C67/52 ,  C07C69/74 ,  C07C211/27 ,  C07C2601/02

摘要： The present invention provides an industrially applicable method for production of a fluorine-containing cyclopropane carboxylic acid compound useful as an intermediate for pharmaceutical and agrichemical products. A fluorine-containing cyclopropane monoester is obtained by: forming a fluorine-containing cyclic sulfate with the use of a fluorine-containing dial compound and sulfuryl fluoride (as a cyclic sulfuric esterification step); reacting the fluorine-containing cyclic sulfate with a malonic diester, thereby forming a fluorine-containing cyclopropane diester (as a cyclopropanation step); and hydrolyzing the fluorine-containing cyclopropane diester (as a hydrolysis step). The fluorine-containing cyclopropane carboxylic acid compound, such as fluorine-containing cyclopropane monoester or its salt, can be obtained with high chemical and optical purity by mixing the fluorine-containing cyclopropane monoester with an amine and subjecting the resulting salt of the fluorine-containing cyclopropane monoester and amine to recrystallization purification.

公开(公告)号：US20180037533A1

公开(公告)日：2018-02-08

申请号：US15551640

申请日：2016-03-15

申请人： CENTRAL GLASS COMPANY, LIMITED

发明人： Takako YAMAZAKI ,  Ryuichi OKAMOTO ,  Akihiro ISHII

IPC分类号： C07C67/307 ,  C07C51/295 ,  C07C69/716 ,  C07C45/67

CPC分类号： C07C67/307 ,  C07C45/676 ,  C07C51/295 ,  C07C69/716 ,  C07C49/16 ,  C07C59/115

摘要： Disclosed is a practical method for production of 3,3-difluoro-2-hydroxypropionic acid, which is important as pharmaceutical and agrichemical intermediates. The method includes forming a 4,4-difluoro-2,2-dichloro-3-oxobutanoic acid ester by reaction of a 4,4-difluoro-3-oxobutanoic acid ester with chlorine (Cl2), forming 3,3-difluoro-1,1-dichloro-2-propanone by reaction of the chlorination product with an acid, and then, reacting the degradation product with a basic aqueous solution.