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1. 发明授权

US06380435B2 PURIFYING PROCESS OF TETRAKIS(FLUOROARYL)BORATE.MAGNESIUM HALIDE, TETRAKIS(FLUOROARYL)BORATE·ETHER COMPLEX AND PRODUCING PROCESS OF THE SAME, AND PRODUCING PROCESS OF TETRAKIS(FLUOROARYL)BORATE DERIVATIVE 有权
标题翻译：（氟）硼酸盐，氟代硼酸盐（氟代）硼酸盐复合物的制备及其制备方法及其制备方法（氟代）硼酸盐衍生物
公开(公告)号：US06380435B2
公开(公告)日：2002-04-30
申请号：US09779673
申请日：2001-02-09
申请人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Yamamoto
发明人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Yamamoto
IPC分类号： C07F502
CPC分类号： C07F5/027
摘要： Tetrakis (fluoroaryl)borate.magnesium halide (Ar4BMgX) expressed by General Formula (1): where each of R1-R10 represents a hydrogen atom, a fluorine atom, a hydrocarbon group, or an alkoxy group, provided that at least one of R1-R5 represents a fluorine atom and at least one of R6-R10 represents a fluorine atom, X represents a chlorine atom, a bromine atom, or an iodide atom, and n represents 2 or 3, is treated with alkali metal salts of carboxylic acid and/or alkali earth metal salts of carboxylic acid. Then, a tetrakis(fluoroaryl)borate derivative (Ar4BZ) is produced by reacting treated Ar4BMgX with a compound generating monovalent cation seeds (for example, N,N-dimethylaniline.hydrochloride). Consequently, it has become possible to provide a purifying process of separating/removing impurities from Ar4BMgX readily and efficiently, and a process of producing inexpensive Ar4BX efficiently.
摘要翻译：由通式（1）表示的四（氟化芳基）硼酸镁卤化物（Ar4BMgX）：其中R1-R10各自表示氢原子，氟原子，烃基或烷氧基，条件是R1 -R5表示氟原子，R6-R10中的至少一个表示氟原子，X表示氯原子，溴原子或碘原子，n表示2或3，用羧酸的碱金属盐处理和/或羧酸的碱土金属盐。然后，通过使处理的Ar4BMgX与产生一价阳离子种子（例如N，N-二甲基苯胺盐酸盐）的化合物反应来制备四（氟化芳基）硼酸盐衍生物（Ar4BZ）。因此，可以容易且高效地提供从Ar4BMgX中分离除去杂质的净化方法，以及有效地制造廉价的Ar4BX的工序。

2. 发明授权

US06624329B2 PURIFYING PROCESS OF TETRAKIS (FLUOROARYL) BORATE·MAGNESIUM HALIDE, TETRAKIS (FLUOROARYL) BORATE·ETHER COMPLEX AND PRODUCING PROCESS OF THE SAME, AND PRODUCING PROCESS OF TETRAKIS (FLUOROARYL) BORATE DERIVATIVE 失效
标题翻译：（氟）硼酸盐，氟代硼酸盐（氟代）硼酸盐复合物的制备及其制备方法及其制备方法（氟代）硼酸盐衍生物
公开(公告)号：US06624329B2
公开(公告)日：2003-09-23
申请号：US10024306
申请日：2001-12-21
申请人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Yamamoto
发明人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Yamamoto
IPC分类号： C07F502
CPC分类号： C07F5/027
摘要： Tetrakis(fluoroaryl)borate•magnesium halide (Ar4BMgX) expressed by General Formula (1): where each of R1-R10 represents a hydrogen atom, a fluorine atom, a hydrocarbon group, or an alkoxy group, provided that at least one of R1-R5 represents a fluorine atom and at least one of R6-R10 represents a fluorine atom, X represents a chlorine atom, a bromine atom, or an iodide atom, and n represents 2 or 3, is treated with alkali metal salts of carboxylic acid and/or alkali earth metal salts of carboxylic acid. Then, a tetrakis(fluoroaryl)borate derivative (Ar4BZ) is produced by reacting treated Ar4BMgX with a compound generating monovalent cation seeds (for example, N,N-dimethylaniline•hydrochloride). Consequently, it has become possible to provide a purifying process of separating/removing impurities from Ar4BMgX readily and efficiently, and a process of producing inexpensive Ar4BX efficiently.
摘要翻译：由通式（1）表示的四（氟化芳基）硼酸镁卤化物（Ar4BMgX）：其中R1-R10各自表示氢原子，氟原子，烃基或烷氧基，条件是R 1 -R5表示氟原子，R6-R10中的至少一个表示氟原子，X表示氯原子，溴原子或碘原子，n表示2或3，用羧酸的碱金属盐处理和/或羧酸的碱土金属盐。然后，通过使处理的Ar4BMgX与产生一价阳离子种子（例如N，N-二甲基苯胺盐酸盐）的化合物反应来制备四（氟化芳基）硼酸盐衍生物（Ar4BZ）。因此，可以容易且高效地提供从Ar4BMgX中分离除去杂质的净化方法，以及有效地制造廉价的Ar4BX的工序。

3. 发明授权

US06215025B1 Method for purifying tetrakis (fluoroaryl) borate/magnesium halide, tetrakis (fluoroaryl) borate/ether complex and process for preparing the same, and process for preparing tetrakis (fluoroaryl) borate derivative 有权
标题翻译：四（氟化芳基）硼酸盐/卤化镁，四（氟化芳基）硼酸盐/醚络合物及其制备方法的纯化方法以及四（氟化芳基）硼酸盐衍生物的制备方法
公开(公告)号：US06215025B1
公开(公告)日：2001-04-10
申请号：US09171832
申请日：1998-10-26
申请人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Yamamoto
发明人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Yamamoto
IPC分类号： C07F502
CPC分类号： C07F5/027
摘要： Tetrakis(fluoroaryl)borate.magnesium halide (Ar4BMgX) expressed by General Formula (1): where each of R1-R10 represents a hydrogen atom, a fluorine atom, a hydrocarbon group, or an alkoxy group, provided that at least one of R1-R5 represents a fluorine atom and at least one of R6-R10 represents a fluorine atom, X represents a chlorine atom, a bromine atom, or an iodide atom, and n represents 2 or 3, is treated with alkali metal salts of carboxylic acid and/or alkali earth metal salts of carboxylic acid. Then, a tetrakis(fluoroaryl)borate derivative (Ar4BZ) is produced by reacting treated Ar4BMgX with a compound generating monovalent cation seeds (for example, N,N-dimethylaniline.hydrochloride). Consequently, it has become possible to provide a purifying process of separating/removing impurities from Ar4BMgX readily and efficiently, and a process of producing inexpensive Ar4BX efficiently.
摘要翻译：由通式（1）表示的四（氟化芳基）硼酸镁卤化物（Ar4BMgX）：其中R1-R10各自表示氢原子，氟原子，烃基或烷氧基，条件是R1 -R5表示氟原子，R6-R10中的至少一个表示氟原子，X表示氯原子，溴原子或碘原子，n表示2或3，用羧酸的碱金属盐处理和/或羧酸的碱土金属盐。然后，通过使处理的Ar4BMgX与产生一价阳离子种子（例如N，N-二甲基苯胺盐酸盐）的化合物反应来制备四（氟化芳基）硼酸盐衍生物（Ar4BZ）。因此，可以容易且高效地提供从Ar4BMgX中分离除去杂质的净化方法，以及有效地制造廉价的Ar4BX的工序。

4. 发明授权

US6118026A Stabilizer for (fluoroaryl)borane compound and methods of stabilizing and crystallizing (fluoroaryl)borane compound 失效
标题翻译：（氟化芳基）硼烷化合物的稳定剂和稳定和结晶（氟化芳基）硼烷化合物的方法
公开(公告)号：US6118026A
公开(公告)日：2000-09-12
申请号：US104042
申请日：1998-06-25
申请人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Yamamoto
发明人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Yamamoto
IPC分类号： C07F5/02 , C07C5/02
CPC分类号： C07F5/027
摘要： A (fluoroaryl)borane compound expressed by General Formula (1): ##STR1## where each of R.sub.1 -R.sub.5 represents a hydrogen atom, a fluorine atom, a hydrocarbon group, or an alkoxy group, provided that at least one of R.sub.1 -R.sub.5 represents a fluorine atom, X represents a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom, and n represents 2 or 3, is stabilized by letting inorganic metal salts having a fluorine atom coexist with the (fluoroaryl)borane compound in a hydrocarbon solution. After the hydrocarbon solution is concentrated in the presence of the inorganic metal salts, the inorganic metal salts are removed and the fluoroaryl)borane compound is crystallized. Consequently, it has become possible to provide a method of stabilizing a (fluoroaryl)borane compound by suppressing the decomposition reaction while the solution is heated and concentrated, stored (preserved), or transported/transferred, and a crystallizing method of isolating highly-pure crystals (powders) of the (fluoroaryl)borane compound efficiently.
摘要翻译：由通式（1）表示的（氟化芳基）硼烷化合物：其中R 1 -R 5各自表示氢原子，氟原子，烃基或烷氧基，条件是R 1 -R 5中的至少一个表示氟原子，X表示氟原子，氯原子，溴原子或碘原子，n表示2或3，通过使具有氟原子的无机金属盐与（氟化芳基）硼烷化合物在烃中共存而稳定化解。在无机金属盐存在下将烃溶液浓缩后，除去无机金属盐，并使氟代芳基）硼烷化合物结晶。因此，可以提供一种通过在将溶液加热浓缩，储存（保存）或输送/转移的同时抑制分解反应来稳定（氟化芳基）硼烷化合物的方法，以及分离高纯度（氟化芳基）硼烷化合物的结晶（粉末）有效。

5. 发明授权

US06410810B1 Handling method of (fluoroaryl) borane compound and preparing method of hydrocarbon solution 失效
标题翻译：（氟化芳基）硼烷化合物的处理方法和烃溶液的制备方法
公开(公告)号：US06410810B1
公开(公告)日：2002-06-25
申请号：US09512289
申请日：2000-02-24
申请人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Hirano
发明人： Hitoshi Mitsui , Tsunemasa Ueno , Ikuyo Ikeno , Naoko Hirano
IPC分类号： C07C720
CPC分类号： C07F5/02 , C07F5/027
摘要： A mixture of bis- and tris(fluoroaryl)borane compounds expressed by General Formula (1) below is handled in the form of a slurry made with a hydrocarbon solvent: where each of R1, R2, R3, R4 and R5 independently represents a hydrogen atom, a fluorine atom, a hydrocarbon group, or an alkoxy group provided that at least one of R1-R5 represents a fluorine atom, X represents a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom, and wherein n represents 2 for the bis(fluoroaryl)borane compounds and 3 for the tris(fluoroaryl)borane compounds. Then, a hydrocarbon solution of the (fluoroaryl)borane compounds having a concentration of the tris(fluoroaryl)borane compounds in a range between 1 wt % and 1 wt % is prepared by dissolving the slurry into a hydrocarbon solvent in a virtually air-tight vessel. Consequently, it has become possible to provide a method of handling the tris(fluoroaryl)borane compounds in an industrially and economically advantageous manner, and a method of preparing the hydrocarbon solution of the tris(fluoroaryl)borane compounds readily and quickly without lowering the purity.
摘要翻译：由以下通式（1）表示的双 - 和三（氟芳基）硼烷化合物的混合物以用烃溶剂制备的浆料的形式进行处理：其中R1，R2，R3，R4和R5各自独立地表示氢原子，氟原子，烃基或烷氧基，只要R 1 -R 5中的至少一个表示氟原子，X表示氟原子，氯原子，溴原子或碘原子，并且其中n 对于双（氟芳基）硼烷化合物，代表2，三（氟芳基）硼烷化合物为3。然后，将具有1重量％至1重量％范围内的三（氟芳基）硼烷化合物浓度的（氟化芳基）硼烷化合物的烃溶液通过将该浆料实际上气密地船只。因此，可以以工业上和经济上有利的方式提供三（氟化芳基）硼烷化合物的处理方法，以及容易且快速地制备三（氟芳基）硼烷化合物的烃溶液而不降低纯度的方法。

6. 发明授权

US6057480A Process for preparing fluoroaryl magnesium derivative and process for preparing (fluoroaryl) borane compound 失效
标题翻译：制备氟芳基镁衍生物的方法和制备（氟化芳基）硼烷化合物的方法
公开(公告)号：US6057480A
公开(公告)日：2000-05-02
申请号：US930708
申请日：1997-10-16
申请人： Tsunemasa Ueno , Ikuyo Katsumi , Naoko Yamamoto , Hitoshi Mitsui
发明人： Tsunemasa Ueno , Ikuyo Katsumi , Naoko Yamamoto , Hitoshi Mitsui
IPC分类号： C07F3/02 , C07F5/02
CPC分类号： C07F3/02 , C07F5/027
摘要： A fluoroaryl magnesium derivative is produced by reacting aryl fluoride, hydrocarbon halide, and magnesium with one another in an ether solvent or a mixed solvent of the ether solvent and a hydrocarbon solvent. Also, a (fluoroaryl)borane compound is produced by mixing both a solution prepared by dissolving the fluoroaryl magnesium derivative into the ether solvent and another solvent prepared by dissolving the boron halide in the ether solvent with a hydrocarbon solvent having a higher boiling point than the ether solvent, so that the fluoroaryl magnesium derivative and boron halide react with each other while the ether solvent is being distilled out.
摘要翻译： PCT No.PCT / JP97 / 00391 Sec。 371日期：1997年10月16日 102（e）日期1997年10月16日PCT 1997年2月12日提交PCT公布。公开号WO97 / 31924 PCT 日期1997年9月4日氟芳基镁衍生物通过芳基氟化物，烃卤化物和镁在醚溶剂或醚溶剂和烃溶剂的混合溶剂中彼此反应来制备。此外，（氟化芳基）硼烷化合物是通过将通过将氟化芳基镁衍生物溶解在醚溶剂中制备的溶液和通过将卤化硼溶解在醚溶剂中制备的另一种溶剂与沸点高于醚溶剂，使得氟化芳基镁衍生物和卤化硼在蒸出醚溶剂的同时彼此反应。

7. 发明授权

US4916233A Method for production of 4-methyl-5-(2-aminoethyl)-thiomethyl)-imidazole 失效
标题翻译： 4-甲基-5-（2-氨基乙基）硫甲基） - 咪唑的制备方法
公开(公告)号：US4916233A
公开(公告)日：1990-04-10
申请号：US342798
申请日：1989-04-25
申请人： Tsunemasa Ueno , Koichi Yamamoto , Masao Kitano , Yutaka Morimoto
发明人： Tsunemasa Ueno , Koichi Yamamoto , Masao Kitano , Yutaka Morimoto
IPC分类号： C07D233/54 , C07D233/64
CPC分类号： C07D233/64 , Y02P20/582
摘要： 4-Methyl-5-[(2-aminoethyl)-thiomethyl]-imidazole can be effectively produced by causing 4-methylimidazole or a salt thereof to react with at least one member selected from the group consisting of (a) a formaldehyde adduct of cysteamine, (b) 2-aminoethanethiol sulfuric acid and formaldehyde or a formaldehyde oligomer, and (c) thiazolidine or a salt thereof, in the presence of a mineral acid, removing a portion of reaction liquid out of the reaction system while maintaining molar concentration of 4-methyl-5-[(2-aminoethyl)-thiomethyl]-imidazole in the reaction system not exceeding 70 mol % based on total mol numbers of 4-methylimidazole and 4-methyl-5-[(2-aminoethyl)-thiomethyl]-imidazole, then separating a liquid containing 4-methyl-5-[(2-aminoethyl)-thiomethyl]-imidazole from the removed portion of reaction liquid, and recycling the remainder into the reaction system.

8. 发明授权

US06187958B1 Amino group-containing thiols and method for production thereof 失效
标题翻译：含氨基硫醇及其制备方法
公开(公告)号：US06187958B1
公开(公告)日：2001-02-13
申请号：US09058729
申请日：1998-04-10
申请人： Takashi Tomita , Tsunemasa Ueno , Daniel Bernard
发明人： Takashi Tomita , Tsunemasa Ueno , Daniel Bernard
IPC分类号： C07C32100
CPC分类号： C07C323/25
摘要： These amino group-containing mono- or dithiols are represented by formula (I). In order to prepare them, ethylene sulfide is reacted with at least one compound of formula (II), the average number of moles of ethylene sulfide added corresponding to the total m+n, and possibly the compound of formula (I) as obtained is further reacted with ethylene sulfide in order to increase the value of m+n. R1 stands for a straight or branched alkyl or alkenyl group having 10 to 30 carbon atoms; R2 stands for a straight or branched alkyl or alkenyl group having 10 to 30 carbon atoms, or a —(CH2—CH2—S)n—H group; m and n, which are identical or different, each represent 0 or an integer in the range of 1 to 10 and satisfy 1.6≦m+n≦20; R′2 stands for a hydrogen atom in which case R2 in formula (I) will represent —(CH2—CH2—S)n—H, or a straight or branched alkyl or alkenyl group having 10 to 30 carbon atoms, in which case it will remain unchanged in the compound of the formula (I).
摘要翻译：这些含氨基的单或二硫醇由式（I）表示。为了制备它们，环硫乙烷与至少一种式（II）的化合物反应，相应于总m + n的平均加入的环硫乙烷的摩尔数，以及可能得到的式（I）化合物是进一步与环硫乙烷反应以增加m + n的值.R1代表具有10至30个碳原子的直链或支链烷基或烯基; R2代表具有10-30个碳原子的直链或支链烷基或烯基，或 - （CH2-CH2-S）n-H基; m和n相同或不同，分别表示0或1〜10的整数，满足1.6≤m+ n <20。 R'2代表氢原子，其中式（I）中的R 2表示 - （CH 2 -CH 2 -S）n H或具有10至30个碳原子的直链或支链烷基或烯基，在这种情况下在式（I）化合物中保持不变。

9. 发明授权

US08501873B2 Water absorbent material, method for production of surface cross-linked water absorbent resin, and method for evaluation of water absorbent material 有权
标题翻译：吸水材料，表面交联吸水性树脂的制造方法以及吸水材料的评价方法
公开(公告)号：US08501873B2
公开(公告)日：2013-08-06
申请号：US11660758
申请日：2005-08-31
申请人： Masazumi Sasabe , Kenji Kadonaga , Shigeru Sakamoto , Motohiro Imura , Tsunemasa Ueno , Hiroko Ueda , Yoshifumi Adachi
发明人： Masazumi Sasabe , Kenji Kadonaga , Shigeru Sakamoto , Motohiro Imura , Tsunemasa Ueno , Hiroko Ueda , Yoshifumi Adachi
IPC分类号： C08F8/42 , C08F8/12 , C08F6/02
CPC分类号： C08J3/248 , C08J3/243 , C08J2300/14 , Y10T428/254 , Y10T428/2982
摘要： A homogeneously surface cross-linked water absorbent resin and a method for the production thereof are provided.The water absorbent material is formed of a surface cross-linked water absorbent resin resulting from granular irregularly pulverized shaped surface cross-linking the product of partial neutralization or whole neutralization of a water absorbent resin having acrylic acid or a metal salt thereof as a main component, which water absorbent material shows a metal atom concentration on the surface of the water absorbent material in the range of 0-10% within 0 second of polishing and 2-35% at 10 seconds value of polishing as determined by subjecting the water absorbent material to Ar ion discharge polishing under a voltage of 500 Å. The surface cross-linked water absorbent resin to be used herein can be produced by surface cross-linking a water absorbent resin having a specific particle diameter with a surface cross-linking agent having a water concentration in a specific range.
摘要翻译：提供均匀的表面交联型吸水性树脂及其制造方法。吸水材料由表面交联的吸水性树脂形成，该表面交联的吸水性树脂是由具有丙烯酸或其金属盐作为主要成分的吸水性树脂的部分中和或全部中和产生的颗粒不规则粉碎的表面交联而成的该吸水材料在抛光的0秒内在吸水材料的表面上表现出0-10％的范围内的金属原子浓度，在10秒的抛光时间为2-35％，通过使吸水材料在500的电压下进行Ar离子放电研磨。这里使用的表面交联型吸水性树脂可以通过将具有特定粒径的吸水性树脂与具有特定范围的水分浓度的表面交联剂进行表面交联来制造。

10. 发明授权

US4785122A Method for production of amine compound 失效
标题翻译：胺化合物的制备方法
公开(公告)号：US4785122A
公开(公告)日：1988-11-15
申请号：US119055
申请日：1987-11-10
申请人： Tsunemasa Ueno , Yutaka Morimoto
发明人： Tsunemasa Ueno , Yutaka Morimoto
IPC分类号： C07D307/52
CPC分类号： C07D307/52
摘要： A method for the producing 2-[[[5-(dialkylamino)alkyl-2-furanyl]methyl]thio]-ethane amine by the reaction of cysteamine or cysteamine hydrochloride containing free hydrogen chloride with 5-(dialkyl amino)alkyl furfuryl alcohol, which method can be obtained the product in a highly yield by carrying out said reaction at a temperature in the range of 30.degree. to 80.degree. C.
摘要翻译：含有游离氯化氢的半胱胺或半胱胺盐酸盐与5-（二烷基氨基）烷基糠醇的反应制备2 - [[[（5-（二烷基氨基）烷基-2-呋喃基]甲基]硫基] - 乙胺的方法通过在30℃〜80℃的温度下进行上述反应，可以高产率地获得该方法。

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