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    Process for production of sulfoxide derivatives or salts thereof in the amorphous state
    1.
    发明申请
    Process for production of sulfoxide derivatives or salts thereof in the amorphous state 审中-公开
    以非晶态生产亚砜衍生物或其盐的方法

    公开(公告)号：US20060178406A1

    公开(公告)日：2006-08-10

    申请号：US10546994

    申请日：2004-03-17

    申请人： Masahiko Tsujii ,  Yukio Morita

    发明人： Masahiko Tsujii ,  Yukio Morita

    IPC分类号： A61K31/4439 ,  C07D403/02

    CPC分类号： C07D401/12

    摘要： A process for producing sulfoxide derivatives or salts thereof in the amorphous state, characterized by heat-drying solvated crystals of a sulfoxide derivative or a salt thereof represented by the general formula (I): wherein R1 represents a hydrogen atom, a methoxy group, or a difluoromethoxy group; R2 represents a methyl group or a methoxy group; R3 represents a 3-methoxypropoxy group, a methoxy group, or a 2,2,2-trifluoroethoxy group; R4 represents a hydrogen atom or a methoxy group; and B represents a hydrogen atom, an alkali metal or ½ alkaline earth metal.

    摘要翻译： 一种制备无定形状态的亚砜衍生物或其盐的方法，其特征在于将由通式（I）表示的亚砜衍生物或其盐的溶剂化晶体加热干燥：其中R 1表示 氢原子，甲氧基或二氟甲氧基; R 2表示甲基或甲氧基; R 3表示3-甲氧基丙氧基，甲氧基或2,2,2-三氟乙氧基; R 4表示氢原子或甲氧基; B表示氢原子，碱金属或½碱土金属。

    Process for production of sulfoxide derivatives or salts thereof in the amorphous state
    2.
    发明授权
    Process for production of sulfoxide derivatives or salts thereof in the amorphous state 失效
    在非晶状态下生产亚砜衍生物或其盐的方法

    公开(公告)号：US07754887B2

    公开(公告)日：2010-07-13

    申请号：US11939418

    申请日：2007-11-13

    申请人： Masahiko Tsujii ,  Yukio Morita

    发明人： Masahiko Tsujii ,  Yukio Morita

    IPC分类号： C07D401/12

    CPC分类号： C07D401/12

    摘要： Process for producing sulfoxide derivatives or salts thereof in the amorphous state, characterized by heat-drying solvated crystals of a sulfoxide derivative or a salt thereof represented by the general formula (I): wherein R1 represents a hydrogen atom, a methoxy group, or a difluoromethoxy group; R2 represents a methyl group or a methoxy group; R3 represents a 3-methoxypropoxy group, a methoxy group, or a 2,2,2-trifluoroethoxy group; R4 represents a hydrogen atom or a methoxy group; and B represents a hydrogen atom, an alkali metal or ½ alkaline earth metal.

    摘要翻译： 制备无定形状态的亚砜衍生物或其盐的方法，其特征在于加热干燥由通式（I）表示的亚砜衍生物或其盐的溶剂化晶体：其中R1表示氢原子，甲氧基或 二氟甲氧基 R2表示甲基或甲氧基; R3表示3-甲氧基丙氧基，甲氧基或2,2,2-三氟乙氧基; R4表示氢原子或甲氧基; B表示氢原子，碱金属或½碱土金属。

    Sulfoxide compounds and acetone complexes, and a process for producing the same
    5.
    发明授权
    Sulfoxide compounds and acetone complexes, and a process for producing the same 有权
    亚砜化合物和丙酮络合物及其制备方法

    公开(公告)号：US06180652B2

    公开(公告)日：2001-01-30

    申请号：US09433786

    申请日：1999-11-03

    申请人： Masahiko Tsujii ,  Nobuo Niikawa ,  Keizo Takayanagi ,  Shigeharu Nochi

    发明人： Masahiko Tsujii ,  Nobuo Niikawa ,  Keizo Takayanagi ,  Shigeharu Nochi

    IPC分类号： A61K3144

    CPC分类号： C07D401/12

    摘要： The present invention provides acetone complexes of sulfoxide compounds, useful as medicines such as inhibitors of gastric acid secretion and anti-ulcer agents or as intermediates for production of medicines, a process for producing the same and a purification method of using the same. Namely, it is the acetone complexes of sulfoxide compounds or of pharmaceutically acceptable salts thereof represented by the following formula: (wherein R1 represents a hydrogen atom, a methoxy group or a difluoromethoxy group, R2 represents a methyl group or a methoxy group, R3 represents a 3-methoxypropoxy group, a methoxy group or a 2,2,2-trifluoroethoxy group, R4 represents a hydrogen atom or a methyl group, n and m independently represent an integer of 1 to 4, and B represents a hydrogen atom, an alkali metal atom or ½ alkaline earth metal atom), which are obtained by treating the sulfoxide compounds or pharmaceutically acceptable salts thereof with acetone.

    摘要翻译： 本发明提供了可用作胃酸分泌抑制剂和抗溃疡剂等药物的亚砜化合物的丙酮配合物，或作为制造药物的中间体的方法及其使用方法。名义上， 它是由下式表示的亚砜化合物或其药学上可接受的盐的丙酮络合物：其中R1表示氢原子，甲氧基或二氟甲氧基，R2表示甲基或甲氧基，R3表示3 - 甲氧基丙氧基，甲氧基或2,2,2-三氟乙氧基，R4表示氢原子或甲基，n和m独立地表示1〜4的整数，B表示氢原子，碱金属 原子或½碱土金属原子），其通过用丙酮处理亚砜化合物或其药学上可接受的盐而获得。

    Methods for producing cyclic benzamidine derivatives
    6.
    发明授权
    Methods for producing cyclic benzamidine derivatives 失效
    环苯甲脒衍生物的制备方法

    公开(公告)号：US07375236B2

    公开(公告)日：2008-05-20

    申请号：US11208289

    申请日：2005-08-18

    申请人： Naoyuki Shimomura ,  Manabu Sasho ,  Akio Kayano ,  Kazuhiro Yoshizawa ,  Masahiko Tsujii ,  Hiroshi Kuroda ,  Ken Furukawa

    发明人： Naoyuki Shimomura ,  Manabu Sasho ,  Akio Kayano ,  Kazuhiro Yoshizawa ,  Masahiko Tsujii ,  Hiroshi Kuroda ,  Ken Furukawa

    IPC分类号： C07D265/30 ,  C07D209/44 ,  C07C43/307

    CPC分类号： C07D295/096 ,  C07C43/225 ,  C07C43/315 ,  C07C255/54 ,  C07C255/56 ,  C07C303/28 ,  C07D209/44 ,  C07D209/48 ,  C07C309/66

    摘要： In the present invention, the methods of producing a fluorinated cyclic benzamidine derivative (A), or a salt thereof, comprise the step of reacting a specific novel compound with ammonia or imide.The methods of this invention for producing a morpholine-substituted phenacyl derivative (B), or a salt thereof, comprise reaction of a specific novel compound with morpholine, reaction of the product with a halogenating reagent, and deketalization of the product.The methods of this invention for a producing cyclic benzamidine derivative (C), or a salt thereof, comprise the step of coupling compound (A), or a salt thereof, with compound (B), or a salt thereof, in the presence of an ether or a hydrocarbon.The methods of this invention for recrystallizing a cyclic benzamidine derivative (C), or a salt thereof, comprise the steps of dissolving compound (C), or the salt thereof, in a mixed solvent comprising an alcohol and water, or a mixed solvent comprising an ether and water, and after dissolution, adding additional water to precipitate crystals of compound (C), or the salt thereof.

    摘要翻译： 在本发明中，制备氟化环状苯甲脒衍生物（A）或其盐的方法包括使特定的新化合物与氨或酰亚胺反应的步骤。 本发明用于生产吗啉取代的苯甲酰甲基衍生物（B）或其盐的方法包括特异性新化合物与吗啉的反应，产物与卤化试剂的反应和产物的脱缩合作用。 本发明的制备环状苯甲脒衍生物（C）或其盐的方法包括将化合物（A）或其盐与化合物（B）或其盐偶联的步骤在 醚或烃。 本发明用于环状苄脒衍生物（C）或其盐的重结晶的方法包括将化合物（C）或其盐溶解在包含醇和水的混合溶剂中的步骤或包含 醚和水，溶解后加入另外的水，使化合物（C）的结晶或其盐析出。

    Protected aminothiazolylacetic acid derivatives
    8.
    发明授权
    Protected aminothiazolylacetic acid derivatives 失效
    受保护的氨基噻唑乙酸衍生物

    公开(公告)号：US5665888A

    公开(公告)日：1997-09-09

    申请号：US412190

    申请日：1995-03-28

    申请人： Yoshio Urawa ,  Akihiko Shimotani ,  Takeo Kanai ,  Masahiko Tsujii

    发明人： Yoshio Urawa ,  Akihiko Shimotani ,  Takeo Kanai ,  Masahiko Tsujii

    IPC分类号： C07D277/20 ,  C07D277/38 ,  C07D277/40 ,  C07D277/42 ,  C07D499/08 ,  C07D501/00 ,  C07D501/06 ,  C07D501/34

    CPC分类号： C07D277/587 ,  C07D277/20 ,  C07D277/42 ,  C07D501/00 ,  Y02P20/55

    摘要： Described is a protected aminothiazolylacetic acid derivative represented by the following formula (I): ##STR1## wherein A represents a nitrogen atom or a methine group, R.sup.1 and R.sup.2 may be the same or different and individually represent a hydrogen atom, a lower alkyl group or a substituted or unsubstituted aryl group, R.sup.3 represents a lower alkoxy group, a halogenated lower alkoxy group, a triphenylmethoxy group, a lower alkyl group or an acyloxy group, and R.sup.4 represents a halogen atom, a hydroxy group, a lower alkoxy group or a substituted or unsubstituted amino group; and salts thereof; as well as processes for the preparation thereof. The protected aminothaizolylacetic acid derivative according to the present invention is an useful intermediate for introducing a 2-(2-aminothiazol-4-yl)-2-alkoxyiminoacetyl group or a 2-(2-aminotiazol-4-yl)-2-alkenoyl group into a cephem skeleton.

    摘要翻译： 描述了由下式（I）表示的受保护的氨基噻唑乙酸衍生物：其中A表示氮原子或次甲基，R 1和R 2可以相同或不同，各自表示氢原子，低级烷基 或取代或未取代的芳基，R3表示低级烷氧基，卤代低级烷氧基，三苯基甲氧基，低级烷基或酰氧基，R4表示卤素原子，羟基，低级烷氧基或 取代或未取代的氨基; 及其盐; 以及其制备方法。 根据本发明的受保护的氨基噻唑乙酸衍生物是用于将2-（2-氨基噻唑-4-基）-2-烷氧基亚氨基乙酰基或2-（2-氨基噻唑-4-基）-2-烯酰基 组成一个头发骨架。

    Purification method of crude product
    10.
    发明授权
    Purification method of crude product 失效
    粗产品纯化方法

    公开(公告)号：US5547580A

    公开(公告)日：1996-08-20

    申请号：US408185

    申请日：1995-03-22

    申请人： Masahiko Tsujii ,  Hirofumi Kuroda ,  Yoshikazu Furusawa ,  Katsuhiko Hirota

    发明人： Masahiko Tsujii ,  Hirofumi Kuroda ,  Yoshikazu Furusawa ,  Katsuhiko Hirota

    IPC分类号： G01N30/26 ,  B01D15/00 ,  B01D15/08

    CPC分类号： B01D15/426

    摘要： Disclosed herein is a purification method of a crude product by column chromatography on silica gel or on a vinyl alcohol copolymer. Methanol-containing n-hexane and/or n-hexane-containing methanol is used as an eluent to elute the crude product, thereby obtaining an intended product with high purity and good yield. The solvents recovered from the effluent can be regenerated without any trouble such as rectification and a great cost by mixing them under stirring and then separating the resulting upper and lower layer from each other. The column used can also be reused again and again by washing with methanol. The separation and purification method is excellent in separation efficiency, operation efficiency and economical efficiency.

    摘要翻译： 本文公开了通过硅胶柱色谱法或乙烯醇共聚物的粗产物的纯化方法。 使用含甲醇的正己烷和/或正己烷的甲醇作为洗脱剂洗脱粗产物，从而获得高纯度和良好产率的预期产物。 从流出液中回收的溶剂可以在没有任何问题（例如精馏）的情况下再生，并且通过在搅拌下将它们混合，然后将得到的上层和下层彼此分离而成本高。 使用的色谱柱也可以通过用甲醇洗涤而一次又一次地使用。 分离纯化方法分离效率高，运行效率高，经济效益好。