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1. 发明授权

US06239293B1 Process for producing dikegulac, its salts and derivatives 失效
标题翻译：生产dikegulac，其盐和衍生物的方法
公开(公告)号：US06239293B1
公开(公告)日：2001-05-29
申请号：US09511508
申请日：2000-02-23
申请人： Lowell J. Lawrence , Stefan Kwiatkowski , Steven G. Mobley
发明人： Lowell J. Lawrence , Stefan Kwiatkowski , Steven G. Mobley
IPC分类号： C07D49314
CPC分类号： C07D493/14
摘要： Dikegulac, its salts and related derivatives are prepared by reacting 2-Keto-L-gulonic acid with 2,2 dimethoxypropane at an elevated temperature in the presence of a catalytic amount of a strong acid. This produces a reaction intermediate which is then reacted with a base to complete hydrolysis and produce an acid salt of dikegulac. Simple concentration and phase separation techniques are used to provide a more efficient, environmentally friendly and cost effective process.
摘要翻译：通过使2-酮-L-古洛糖酸与2,2-二甲氧基丙烷在升高的温度下在催化量的强酸存在下反应来制备二酮酸，其盐和相关衍生物。这产生反应中间体，然后将其与碱反应以完成水解并产生dikegulac的酸式盐。使用简单的浓缩和相分离技术来提供更有效，环保且具有成本效益的方法。

2. 发明授权

US6137009A Method of manufacturing flumetralin 有权
标题翻译：氟美他啶的制备方法
公开(公告)号：US6137009A
公开(公告)日：2000-10-24
申请号：US416543
申请日：1999-10-12
申请人： Stefan Kwiatkowski , Steven G. Mobley , Kryzsztof Pupek , Miroslaw Golinski , Paul D. Smith
发明人： Stefan Kwiatkowski , Steven G. Mobley , Kryzsztof Pupek , Miroslaw Golinski , Paul D. Smith
IPC分类号： C07C209/08 , C07C211/29 , C07C209/00
CPC分类号： C07C209/08
摘要： The invention is a process to manufacture the intermediate secondary amine N-ethyl-2-chloro-6-fluoro-benzylamine, and then the process of reacting this intermediate to manufacture the herbicide flumetralin. Equimolar quantities of monoethylamine, sodium hydroxide, and 2-chloro-6-fluorobenzyl chloride are reacted at a temperature between about 70.degree. C. and about 100.degree. C. in a composition containing at least 2.5 times the required quantity of monoethylamine. The reagent monoethylamine functions as solvent and heat sink for the reaction, and also minimizes the formation of undesired byproducts. The excess monoethylamine is removed after formation of the intermediate. Then, equimolar quantities of sodium hydroxide in water and molten 4-chloro-3-5-dinitrobenzotrifluoride are added to the intermediate, and the temperature is controlled between about 90.degree. C. and about 115.degree. C. The product of this reaction is relatively pure, i.e., 98 percent by weight, molten flumetralin. It is advantageous to wash the product with boiling water to facilitate removal of salt and excess sodium hydroxide.
摘要翻译：本发明是制备中间仲胺N-乙基-2-氯-6-氟 - 苄胺的方法，然后是使该中间体反应以制备除草剂氟马特林的方法。将等摩尔量的单乙胺，氢氧化钠和2-氯-6-氟苄基氯在约70℃至约100℃的温度下在含有至少2.5倍所需量的单乙胺的组合物中反应。试剂单乙胺用作反应的溶剂和散热器，并且还使不期望的副产物的形成最小化。在形成中间体之后除去过量的单乙胺。然后，将等摩尔量的氢氧化钠水溶液和熔融的4-氯-3,5-二硝基三氟甲苯加入到中间体中，温度控制在约90℃至约115℃之间。该反应的产物相对纯的，即98重量％的熔融氟汞。用沸水洗涤产品以便于除去盐和过量的氢氧化钠是有利的。

3. 发明授权

US5689006A Process for producing n-alkyl-dinitroalkylanilines 失效
标题翻译：制备正烷基二硝基烷基苯胺的方法
公开(公告)号：US5689006A
公开(公告)日：1997-11-18
申请号：US496774
申请日：1995-06-29
申请人： Stefan Kwiatkowski , Krzysztof Pupek , Brenda L. Lawrence , Lowell J. Lawrence
发明人： Stefan Kwiatkowski , Krzysztof Pupek , Brenda L. Lawrence , Lowell J. Lawrence
IPC分类号： C07C209/18 , C07C311/39
CPC分类号： C07C209/18
摘要： This invention relates to a process for producing N-alkyl-dinitroalkylaniline and particularly N-sec-butyl-4-tert-butyl-2,6-dinitroaniline by methylation of an alkylphenol followed by nitration of the resulting alkylanisole which is followed by reaction with an amine.
摘要翻译：本发明涉及通过烷基苯酚甲基化制备N-烷基二硝基烷基苯胺，特别是N-仲丁基-4-叔丁基-2,6-二硝基苯胺的方法，然后硝化得到的烷基苯甲醚，随后与胺。

4. 发明授权

US5663441A Production of mono-N-alkyl-dinitroalkylanilines and N-alkyl-dinitroaniline derivatives 失效
标题翻译：单-N-烷基二硝基烷基苯胺和N-烷基二硝基苯胺衍生物的制备
公开(公告)号：US5663441A
公开(公告)日：1997-09-02
申请号：US621286
申请日：1996-03-22
申请人： Stefan Kwiatkowski , Krzysztof Pupek , Brenda L. Lawrence , Lowell J. Lawrence
发明人： Stefan Kwiatkowski , Krzysztof Pupek , Brenda L. Lawrence , Lowell J. Lawrence
IPC分类号： C07C209/18 , C07C303/40
CPC分类号： C07C209/18
摘要： This invention relates to a process for producing mono- and di- N-alkyl-dinitroalkylaniline or dinitroaniline derivative and particularly N-sec-butyl-4-tert-butyl-2,6-dinitroaniline by methylation of an alkylphenol or phenol derivative followed by nitration of the resulting acetic acid alkylanisole or anisole derivative which is followed by reaction with an amine. Acetic acid by-product produced during nitration is recycled by converting back to acetic anhydride.
摘要翻译：本发明涉及通过烷基酚或苯酚衍生物的甲基化制备单 - 和二 - N-烷基二硝基烷基苯胺或二硝基苯胺衍生物，特别是N-仲丁基-4-叔丁基-2,6-二硝基苯胺的方法，硝化所得乙酸烷基苯甲醚或苯甲醚衍生物，然后与胺反应。在硝化过程中产生的乙酸副产物通过转化回乙酸酐进行再循环。

5. 发明授权

US5922913A Process for nitrating aromatic amines 失效
标题翻译：硝化芳香胺的方法
公开(公告)号：US5922913A
公开(公告)日：1999-07-13
申请号：US187949
申请日：1998-11-06
申请人： Lowell J. Lawrence , Stefan Kwiatkowski , Paul D. Smith
发明人： Lowell J. Lawrence , Stefan Kwiatkowski , Paul D. Smith
IPC分类号： C07C209/76 , C07C209/00
CPC分类号： C07C209/76
摘要： Disclosed is a process of nitrating or dinitrating an aromatic amine compound that involves reacting the aromatic amine and nitric acid in the presence of acetic acid such that the molar ratio of the aromatic amine compound to acetic acid is from about 1:2 to about 1:16, and the molar ratio of nitric acid to the aromatic amine is between about 1.0 to about 1.5 times the nitric acid needed to complete the reaction. More particularly, the invention is a process of forming Pendimethalin, N-(1-ethylpropyl)-2,6-dinitro-3,4-xylidine, from N-(1-ethylpropyl)-3,4-xylidine (4-NAX) that involves reacting 4-NAX and nitric acid in the presence of acetic acid such that the molar ratio of nitric to the 4-NAX is between about 2:1 and about 3:1, preferably between about 2:1 and about 2.6:1, and such that the molar ratio of 4-NAX to acetic acid is between about 1:2 to about 1:16, preferably between about 1:4 and about 1:8.
摘要翻译：公开了一种芳族胺化合物的硝化或二硝化方法，其包括在乙酸存在下使芳族胺和硝酸反应，使得芳族胺化合物与乙酸的摩尔比为约1:2至约1:1。 16，硝酸与芳香胺的摩尔比为完成反应所需的硝酸的约1.0至约1.5倍。更具体地说，本发明是由N-（1-乙基丙基）-3,4-二甲苯胺（4-NAX）形成二甲戊灵，N-（1-乙基丙基）-2,6-二硝基-3,4-二甲苯胺的方法），其包括在乙酸存在下使4-NAX和硝酸反应，使得硝酸与4-NAX的摩尔比为约2:1至约3:1，优选约2:1至约2.6:1。 1，使得4-NAX与乙酸的摩尔比为约1:2至约1:16，优选约1:4至约1:8。

6. 发明授权

US5922915A Process for removing N-nitroso compounds from organo-amine compositions including dinitroaniline herbicides 失效
标题翻译：从包括二硝基苯胺除草剂的有机胺组合物中除去N-亚硝基化合物的方法
公开(公告)号：US5922915A
公开(公告)日：1999-07-13
申请号：US76015
申请日：1998-05-11
申请人： Lowell J. Lawrence , Stefan Kwiatkowski
发明人： Lowell J. Lawrence , Stefan Kwiatkowski
IPC分类号： C07C209/84 , C07C211/52 , A01N33/06
CPC分类号： C07C209/84
摘要： A simple and inexpensive process is described for reducing the concentration of N-nitroso-containing compounds. The process is applicable for compositions comprising N-nitroso-containing compounds and other desired compounds wherein the N-nitroso-containing compounds thermally decompose at a temperature below the decomposition temperature of the desired compounds. For compositions comprising N-nitroso-pendimethalin in Pendimethalin, the process requires heating the mixture to a temperature greater than about 120.degree. C., and holding the Pendimethalin at that temperature for a time effective to decompose the N-nitroso-pendimethalin present in the mixture. Volatile decomposition products are advantageously removed from the composition.
摘要翻译：描述了一种简单而廉价的方法来降低含有亚硝基的化合物的浓度。该方法适用于含有N-亚硝基化合物和其它所需化合物的组合物，其中N-亚硝基化合物在低于所需化合物的分解温度的温度下热分解。对于在二甲戊四烯中包含N-亚硝基二甲戊乐灵的组合物，该方法需要将混合物加热至大于约120℃的温度，并将该二甲戊乐灵在该温度下保持一段时间，以有效地分解存在于该物质中的N-亚硝基二甲戊乐灵混合物。挥发性分解产物有利地从组合物中除去。

7. 发明授权

US5777168A Process for producing N-alkyl-dinitroalkylanilines 失效
标题翻译：制备N-烷基 - 二硝基烷基苯胺的方法
公开(公告)号：US5777168A
公开(公告)日：1998-07-07
申请号：US868321
申请日：1997-06-03
申请人： Stefan Kwiatkowski , Krzysztof Pupek , Brenda L. Lawrence , Lowell J. Lawrence
发明人： Stefan Kwiatkowski , Krzysztof Pupek , Brenda L. Lawrence , Lowell J. Lawrence
IPC分类号： C07C209/18
CPC分类号： C07C209/18
摘要： This invention relates to a process for producing N-alkyl-dinitroalkylaniline and particularly N-sec-butyl-4-tert-butyl-2,6-dinitroaniline by methylation of an alkylphenol followed by a one or two stage dinitration of the resulting alkylanisole which is followed by reaction with an amine.
摘要翻译：本发明涉及通过烷基苯酚的甲基化，然后对所得烷基苯甲醚进行一次或两次二硝化制备N-烷基二硝基烷基苯胺，特别是N-仲丁基-4-叔丁基-2,6-二硝基苯胺的方法，然后与胺反应。

8. 发明授权

US5728881A Process for preparing trifluralin 失效
标题翻译：制备氟乐灵的方法
公开(公告)号：US5728881A
公开(公告)日：1998-03-17
申请号：US810883
申请日：1997-03-05
申请人： Stefan Kwiatkowski , Krzysztof Pupek , Miroslaw J. Golinski , Paul D. Smith , Lowell J. Lawrence
发明人： Stefan Kwiatkowski , Krzysztof Pupek , Miroslaw J. Golinski , Paul D. Smith , Lowell J. Lawrence
IPC分类号： C07C205/12 , C07C209/10 , C07C211/48 , C02C209/10
CPC分类号： C07C209/10 , C07C201/12 , Y02P20/582
摘要： A process is provided for preparing 2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)benzenamine from 4-chlorotrifluoromethylbenzene. The process includes a two stage nitration and an amination step. Ethylene dichloride is utilized as a diluent and solvent in the nitration steps. Spent acid from the first nitration is reconstituted with sulfur trioxide for use in the second nitration. Spent acid from the second nitration is used directly in the first nitration and evaporation is used to remove nitrosoamines from the final trifluralin product.
摘要翻译：提供了从4-氯三氟甲基苯制备2,6-二硝基-N，N-二丙基-4-（三氟甲基）苯胺的方法。该方法包括两步硝化和胺化步骤。二氯化乙烯在硝化步骤中用作稀释剂和溶剂。来自第一次硝化的废酸用三氧化硫重新配制用于第二次硝化。来自第二硝化的废酸直接用于第一硝化，蒸发用于从最终的氟乐灵产物中除去亚硝基胺。

9. 发明授权

US5705698A Process for the production of pendimethalin and iso-pendimethalin 失效
标题翻译：生产二甲戊乐灵和异二甲戊乐灵的方法
公开(公告)号：US5705698A
公开(公告)日：1998-01-06
申请号：US621403
申请日：1996-03-25
申请人： Lowell J. Lawrence , Stefan Kwiatkowski , Krzysztof Pupek , Miroslaw J. Golinski
发明人： Lowell J. Lawrence , Stefan Kwiatkowski , Krzysztof Pupek , Miroslaw J. Golinski
IPC分类号： C07C209/22
CPC分类号： C07C209/22
摘要： A process is provided for the preparation of isometrically pure pendimethalin and iso-pendimethalin as well as mixtures thereof.
摘要翻译：提供了用于制备等度纯的二甲戊乐灵和异二甲戊乐灵以及它们的混合物的方法。

10. 发明申请

US20120164234A1 COMPOSITIONS AND METHODS FOR SEPARATING, CHARACTERIZING AND ADMINISTERING SOLUBLE SELENOGLYCOPROTEINS 有权
标题翻译：用于分离，表征和施用可溶性硒蛋白的组合物和方法
公开(公告)号：US20120164234A1
公开(公告)日：2012-06-28
申请号：US13235191
申请日：2011-09-16
申请人： Stefan Kwiatkowski , Ronan Power , Clayton Matney , Paiman Peter Ghoroghchian , Eric Michael Ostertag
发明人： Stefan Kwiatkowski , Ronan Power , Clayton Matney , Paiman Peter Ghoroghchian , Eric Michael Ostertag
IPC分类号： A61K9/14 , A61K38/02 , A23L1/305 , C07K14/39 , C07K1/36 , B82Y99/00 , B82Y5/00
CPC分类号： A61K9/1273 , A61K36/064 , A61K38/00 , C07K14/39
摘要： The invention relates to soluble selenium compositions and methods of production, separation and purification thereof. In particular the present invention provides methods of preparing water soluble selenoglycoproteins (e.g., via extracting selenoglycoproteins from selenium enriched yeast), methods of supplementing a selenium deficient composition via admixing water soluble selenoglycoproteins with the selenium deficient composition, compositions comprising the water soluble selenoglycoproteins and methods of administering the same.
摘要翻译：本发明涉及可溶性硒组合物及其生产，分离和纯化方法。特别地，本发明提供了制备水溶性硒代糖蛋白的方法（例如，通过从富硒酵母提取硒代糖蛋白），通过将水溶性硒代糖蛋白与缺硒组合物混合来补充硒缺乏组合物的方法，包含水溶性硒代糖蛋白的组合物和方法的管理。

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