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1. 发明授权

US06399819B1 Process for purifying creatine 失效
标题翻译：净化肌酸的方法
公开(公告)号：US06399819B1
公开(公告)日：2002-06-04
申请号：US09734028
申请日：2000-12-12
申请人： Knut Kessel , Günter Scherr , Thomas Bogenstätter , Stefan Orsten , Dirk Franke
发明人： Knut Kessel , Günter Scherr , Thomas Bogenstätter , Stefan Orsten , Dirk Franke
IPC分类号： C07C24100
CPC分类号： C07C277/08 , C07C279/14
摘要： A process for purifying creatine is described in which the creatine to be purified in the form free of water of crystallization is introduced into a saturated aqueous solution of creatine monohydrate, in which the creatine free of water of crystallization is dissolved with hydration, crystals of creatine monohydrate precipitate from the aqueous solution and these are separated off from the aqueous solution.
摘要翻译：描述了一种纯化肌酸的方法，其中将没有结晶水形式的要纯化的肌酸引入饱和的肌酸一水合物水溶液中，其中不含结晶水的肌酸水合溶解，肌酸晶体从水溶液中沉淀出一水合物，并将其从水溶液中分离出来。

2. 发明申请

US20110224433A1 Process for Manufacturing Substituted 3-pyridylmethyl Ammonium Bromides 有权
标题翻译：制备取代的3-吡啶基甲基溴化铵的方法
公开(公告)号：US20110224433A1
公开(公告)日：2011-09-15
申请号：US13128787
申请日：2009-11-13
申请人： Joachim Gebhardt , Frederik Menges , Michael Rack , Michael Keil , Jochen Schroeder , Stefan Orsten , Helmut Zech , David Cortes , Robert Leicht , Tony Yegerlehner , Rodney F. Klima
发明人： Joachim Gebhardt , Frederik Menges , Michael Rack , Michael Keil , Jochen Schroeder , Stefan Orsten , Helmut Zech , David Cortes , Robert Leicht , Tony Yegerlehner , Rodney F. Klima
IPC分类号： C07D251/00 , C07D213/80 , C07D237/00 , C07D241/00 , C07D401/04
CPC分类号： C07D401/04 , C07D213/80 , C07D401/06 , C07D403/06 , C07D413/06 , C07D417/06
摘要： A process for manufacturing 5,6-disubstituted-3-pyridylmethyl ammonium bromides (I), wherein Q is a tertiary aliphatic or cyclic, saturated, partially unsaturated or aromatic amine; Z is hydrogen or halogen; Z1 is hydrogen, halogen, cyano or nitro; Y and Y1 are each independently OR1, NR1R2, or when taken together YY1 is —O—, —S— or NR3—; R1 and R2 are each independently hydrogen, C1-C4 alkyl optionally substituted with C1-C4 alkoxy or phenyl optionally substituted with one to three C1-C4 alkyl groups, C1-C4 alkoxy groups or halogen atoms, or phenyl optionally substituted with one to three C1-C4 alkyl groups, C1-C4 alkoxy groups or halogen atoms; R3 is hydrogen or C1-C4 alkyl; comprises the steps of (i) reacting a compound of formula (II), wherein the symbols have the meaning given in formula (I), with bromine in the presence of a radical initiator in a solvent mixture comprising an aqueous phase and an organic phase, where the organic phase comprises a solvent selected from 1,2-dichloroethane, chlorobenzene, 1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichlorobenzene and tetrachloromethane, and where the pH-value of the aqueous phase is from 3 to
摘要翻译：制备5,6-二取代-3-吡啶基甲基溴化铵（I）的方法，其中Q是叔脂族或环状饱和的，部分不饱和的或芳族的胺; Z是氢或卤素; Z1是氢，卤素，氰基或硝基; Y和Y1各自独立地为OR 1，NR 1 R 2，或者当Y Y 1为-O - ， - S-或NR 3 - 时。 R 1和R 2各自独立地为氢，任选被C 1 -C 4烷氧基取代的C 1 -C 4烷基或任选被一至三个C 1 -C 4烷基，C 1 -C 4烷氧基或卤素原子取代的苯基，或任选被一至三个 C1-C4烷基，C1-C4烷氧基或卤原子; R3是氢或C1-C4烷基; 包括以下步骤：（i）在自由基引发剂存在下，将包含式（I）中给出的符号的式（II）化合物与溴在含水相和有机相的溶剂混合物中反应，其中有机相包含选自1,2-二氯乙烷，氯苯，1,2-二氯苯，1,3-二氯苯，1,4-二氯苯和四氯甲烷的溶剂，其中水相的pH值来自 3至<8，得到3-溴甲基-5,6-二取代的吡啶化合物（III），其中Y，Y 1，Z和Z 1具有式（I）中给出的含义，和（ⅱ）使溴化合物式（III）与叔胺碱Q在溶剂中在约0℃至100℃的温度范围内

3. 发明授权

US07145034B2 Method for producing N-phosphonomethylglycine 失效
标题翻译： N-膦酰基甲基甘氨酸的制备方法
公开(公告)号：US07145034B2
公开(公告)日：2006-12-05
申请号：US10481579
申请日：2002-06-21
申请人： Christian Wulff , Stefan Orsten , Alfred Oftring , Peter Zehner
发明人： Christian Wulff , Stefan Orsten , Alfred Oftring , Peter Zehner
IPC分类号： C07F9/22 , C07F9/28
CPC分类号： C07F9/4093 , C07F9/3813
摘要： The invention relates to a process for preparing N-phosphono-methylglycine by reacting a hexahydrotriazine compound with a triacyl phosphite in an organic solvent, hydrolyzing the resulting phosphono compound after prior extraction into an aqueous phase and separation from the organic phase. The process avoids decomposition of the organic solvent during hydrolysis.
摘要翻译：本发明涉及通过在有机溶剂中使六氢三嗪化合物与亚磷酸三辛酯反应制备N-膦酰基 - 甲基甘氨酸的方法，在事先将其萃取到水相中并将其与有机相分离之后水解所得的膦酰基化合物。该方法避免了水解期间有机溶剂的分解。

4. 发明授权

US07071354B2 Method for producing N-phosphonomethylglycine 失效
标题翻译： N-膦酰基甲基甘氨酸的制备方法
公开(公告)号：US07071354B2
公开(公告)日：2006-07-04
申请号：US10481565
申请日：2002-06-21
申请人： Hugues Vandenmersch , Hartwig Voss , Stefan Orsten , Christian Wulff
发明人： Hugues Vandenmersch , Hartwig Voss , Stefan Orsten , Christian Wulff
IPC分类号： C07F9/22 , C07F9/28
CPC分类号： C07F9/3813
摘要： The present invention relates to a process for the recovery of N-phosphonomethylglycine from an aqueous mixture which contains N-phosphonomethylglycine, ammonium halides, and alkali metal or alkaline earth metal halides and optionally organic impurities in dissolved form, where (a) the pH of the mixture is adjusted to a value in the range from 2 to 8, (b) a separation of the mixture on a selective nanofiltration membrane is performed, a retentate which is richer in N-phosphonomethylglycine and poorer in halides and a permeate which is richer in halides and poorer in N-phosphonomethylglycine being obtained, and (c) the N-phosphonomethylglycine is recovered from the retentate. The process according to the invention makes possible the recovery of the N-phosphonomethylglycine with simultaneous separation of the halide salts.
摘要翻译：本发明涉及从含有N-膦酰基甲基甘氨酸，卤化铵和碱金属或碱土金属卤化物和任选的溶解形式的有机杂质的含水混合物中回收N-膦酰基甲基甘氨酸的方法，其中（a）将混合物调节至2至8范围内的值，（b）进行选择性纳滤膜上的混合物分离，更富含N-膦酰基甲基甘氨酸并且较差的卤化物的渗余物和富含物的渗透物在得到的N-膦酰基甲基甘氨酸的卤化物和较差的碱中，和（c）从渗余物中回收N-膦酰基甲基甘氨酸。根据本发明的方法使得可以同时分离卤化物盐来回收N-膦酰基甲基甘氨酸。

5. 发明授权

US06818793B2 Method for production of n-phosphonomethylglycine 失效
标题翻译： n-膦酰基甲基甘氨酸的生产方法
公开(公告)号：US06818793B2
公开(公告)日：2004-11-16
申请号：US10168717
申请日：2002-06-24
申请人： Christian Wulff , Stefan Orsten , Alfred Oftring
发明人： Christian Wulff , Stefan Orsten , Alfred Oftring
IPC分类号： C07F928
CPC分类号： C07F9/4093 , C07F9/3813
摘要： The present invention relates to a process for the preparation of N-phosphonomethylglycine by reacting a hexahydrotriazine derivative with a triacyl phosphite. The process gives N-phosphonomethylglycine in high yield and in a simple and inexpensive manner.
摘要翻译：本发明涉及通过使六氢三嗪衍生物与亚磷酸三酰基酯反应来制备N-膦酰基甲基甘氨酸的方法。该方法以高产率和简单且廉价的方式得到N-膦酰基甲基甘氨酸。

6. 发明授权

US06660878B2 Process for the preparation of N-phosphonomethylglycine 失效
公开(公告)号：US06660878B2
公开(公告)日：2003-12-09
申请号：US10368577
申请日：2003-02-20
申请人： Christian Wulff , Stefan Orsten , Alfred Oftring
发明人： Christian Wulff , Stefan Orsten , Alfred Oftring
IPC分类号： C07F902
CPC分类号： C07F9/4093 , C07F9/3813
摘要： The present invention relates to a process for the preparation of N-phosphonomethylglycine by reacting a hexahydrotriazine derivative with a triacyl phosphite. The process gives N-phosphonomethylglycine in high yield and in a simple and inexpensive manner.

7. 发明授权

US09096570B2 Process for manufacturing substituted 3-pyridylmethyl ammonium bromides 有权
标题翻译：制备取代的3-吡啶基甲基溴化铵的方法
公开(公告)号：US09096570B2
公开(公告)日：2015-08-04
申请号：US13128787
申请日：2009-11-13
申请人： Joachim Gebhardt , Frederik Menges , Michael Rack , Michael Keil , Jochen Schroeder , Stefan Orsten , Helmut Zech , David Cortes , Robert Leicht , Tony Yegerlehner , Rodney F. Klima
发明人： Joachim Gebhardt , Frederik Menges , Michael Rack , Michael Keil , Jochen Schroeder , Stefan Orsten , Helmut Zech , David Cortes , Robert Leicht , Tony Yegerlehner , Rodney F. Klima
IPC分类号： C07D401/06 , C07D403/06 , C07D413/06 , C07D417/06 , C07D213/80 , C07D401/04
CPC分类号： C07D401/04 , C07D213/80 , C07D401/06 , C07D403/06 , C07D413/06 , C07D417/06
摘要： A process for manufacturing 5,6-disubstituted-3-pyridylmethyl ammonium bromides (I), wherein Q is a tertiary aliphatic or cyclic, saturated, partially unsaturated or aromatic amine; Z is hydrogen or halogen; Z1 is hydrogen, halogen, cyano or nitro; Y and Y1 are each independently OR1, NR1R2, or when taken together YY1 is —O—, —S— or NR3—; R1 and R2 are each independently hydrogen, C1-C4 alkyl optionally substituted with C1-C4 alkoxy or phenyl optionally substituted with one to three C1-C4 alkyl groups, C1-C4 alkoxy groups or halogen atoms, or phenyl optionally substituted with one to three C1-C4 alkyl groups, C1-C4 alkoxy groups or halogen atoms; R3 is hydrogen or C1-C4 alkyl; comprises the steps of (i) reacting a compound of formula (II), wherein the symbols have the meaning given in formula (I), with bromine in the presence of a radical initiator in a solvent mixture comprising an aqueous phase and an organic phase, where the organic phase comprises a solvent selected from 1,2-dichloroethane, chlorobenzene, 1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichlorobenzene and tetrachloromethane, and where the pH-value of the aqueous phase is from 3 to
摘要翻译：制备5,6-二取代-3-吡啶基甲基溴化铵（I）的方法，其中Q是叔脂族或环状饱和的，部分不饱和的或芳族的胺; Z是氢或卤素; Z1是氢，卤素，氰基或硝基; Y和Y1各自独立地为OR 1，NR 1 R 2，或者当Y Y 1为-O - ， - S-或NR 3 - 时。 R 1和R 2各自独立地为氢，任选被C 1 -C 4烷氧基取代的C 1 -C 4烷基或任选被一至三个C 1 -C 4烷基，C 1 -C 4烷氧基或卤素原子取代的苯基，或任选被一至三个 C1-C4烷基，C1-C4烷氧基或卤原子; R3是氢或C1-C4烷基; 包括以下步骤：（i）在自由基引发剂存在下，将包含式（I）中给出的符号的式（II）化合物与溴在含水相和有机相的溶剂混合物中反应，其中有机相包含选自1,2-二氯乙烷，氯苯，1,2-二氯苯，1,3-二氯苯，1,4-二氯苯和四氯甲烷的溶剂，其中水相的pH值来自 3至<8，得到3-溴甲基-5,6-二取代的吡啶化合物（III），其中Y，Y 1，Z和Z 1具有式（I）中给出的含义，和（ⅱ）使溴化合物式（III）与叔胺碱Q在溶剂中在约0℃至100℃的温度范围内

8. 发明授权

US06855841B2 Process for the preparation of N-phosphonomethylglycine 失效
标题翻译： N-膦酰基甲基甘氨酸的制备方法
公开(公告)号：US06855841B2
公开(公告)日：2005-02-15
申请号：US10664892
申请日：2003-09-22
申请人： Christian Wulff , Stefan Orsten , Alfred Oftring
发明人： Christian Wulff , Stefan Orsten , Alfred Oftring
IPC分类号： C07F9/38 , C07F9/40 , C07F9/02
CPC分类号： C07F9/4093 , C07F9/3813
摘要： The present invention relates to a process for the preparation of N-phosphonomethylglycine by reacting a hexahydrotriazine derivative with a triacyl phosphite. The process gives N-phosphonomethylglycine in high yield and in a simple and inexpensive manner.
摘要翻译：本发明涉及通过使六氢三嗪衍生物与亚磷酸三酰基酯反应来制备N-膦酰基甲基甘氨酸的方法。该方法以高产率和简单且廉价的方式得到N-膦酰基甲基甘氨酸。

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