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1. 发明授权

US08981079B2 Purification of tertiary formamide contaminated with tertiary acetamide 有权
标题翻译：用叔乙酰胺污染的叔甲酰胺的纯化
公开(公告)号：US08981079B2
公开(公告)日：2015-03-17
申请号：US13378531
申请日：2010-06-18
申请人： James Edwin Wiley, Jr. , Mohamad R. Jaber
发明人： James Edwin Wiley, Jr. , Mohamad R. Jaber
IPC分类号： C07H5/02 , C07C233/03 , C07C231/24 , C07H1/06
CPC分类号： C07C231/24 , C07H1/06 , C07H5/02 , C07C233/03
摘要： A chlorinating agent such as a chloroiminium species is used to remove or neutralize tertiary acetamide present as a contaminant in a tertiary formamide solvent. Tertiary formamide solvent purified or treated in this manner can be used as a reaction vehicle for the chlorination of sucrose-6-acylates, thereby improving the yields of the desired sucralose-6-acylate (an intermediate in the production of sucralose).
摘要翻译：使用氯化剂如氯亚胺鎓物质来除去或中和作为叔甲酰胺溶剂中的污染物存在的叔乙酰胺。以这种方式纯化或处理的叔甲酰胺溶剂可用作蔗糖-6-酰化物氯化反应载体，从而提高所需三氯半乳蔗糖-6-酰化物（三氯蔗糖生产中的中间体）的产率。

2. 发明授权

US08436157B2 Method for the production of sucralose 有权
标题翻译：生产三氯蔗糖的方法
公开(公告)号：US08436157B2
公开(公告)日：2013-05-07
申请号：US12409951
申请日：2009-03-24
申请人： James Edwin Wiley, Jr. , Duane A. Leinhos , David A. Dentel , John Kerr
发明人： James Edwin Wiley, Jr. , Duane A. Leinhos , David A. Dentel , John Kerr
IPC分类号： C07H1/00
CPC分类号： C07H5/02 , C07H1/00
摘要： The present invention provides a method for producing sucralose from a feed stream including a sucrose-6-acylate in a reaction vehicle. The method includes: (i) reacting the sucrose-6-acylate with a chlorinating agent in order to chlorinate the 4, 1′ and 6′ positions of the sucrose-6-acylate; (ii) quenching the product stream of (i) with an aqueous solution of a base to provide a sucralose-6-acylate and the chloride salt of said base, wherein the concentration of the aqueous solution of the base is sufficiently high such that at least a portion of the chloride salt of the base is formed as a precipitate; (iii) either: deacylating the sucralose-6-acylate by treating the product stream of (ii) with a base and thereafter removing precipitated salt to provide a product stream including sucralose; or: removing precipitated salt from the product stream of (ii) and thereafter deacylating the sucralose-6-acylate by treating with a base to provide a product stream including sucralose; and (iv) isolating sucralose from the product stream of (iii).
摘要翻译：本发明提供了在反应载体中从包含蔗糖-6-酰化物的进料流中制备三氯半乳蔗糖的方法。该方法包括：（i）使蔗糖-6-酰化物与氯化剂反应，以使蔗糖-6-酰化物的4,1'和6'位置氯化; （ii）用碱的水溶液淬灭（i）的产物流，得到三氯半乳蔗糖-6-酰化物和所述碱的氯化物盐，其中碱的水溶液的浓度足够高，使得在至少一部分碱的氯化物盐形成沉淀物; （iii）：通过用碱处理（ii）的产物流，然后除去沉淀的盐以提供包含三氯蔗糖的产物流，使三氯蔗糖-6-酰化物脱酰化; 或者：从（ii）的产物流中除去沉淀的盐，然后用碱处理三氯半乳蔗糖-6-酰化物，以提供包含三氯蔗糖的产物流; 和（iv）从（iii）的产物流中分离三氯半乳蔗糖。

3. 发明授权

US08436156B2 Method for the production of sucralose 有权
标题翻译：生产三氯蔗糖的方法
公开(公告)号：US08436156B2
公开(公告)日：2013-05-07
申请号：US12345998
申请日：2008-12-30
申请人： John Kerr , Robert Jansen , Duane A. Leinhos , James Edwin Wiley, Jr. , Sebastien Camborieux , Anthony Baiada , Gordon Walker , Carlo Maffezzoni
发明人： John Kerr , Robert Jansen , Duane A. Leinhos , James Edwin Wiley, Jr. , Sebastien Camborieux , Anthony Baiada , Gordon Walker , Carlo Maffezzoni
IPC分类号： C07H15/00
CPC分类号： C07H1/06 , C07H5/02
摘要： The present invention provides a method for producing sucralose from a feed stream resulting from the chlorination of a sucrose-6-acylate in a reaction vehicle. The feed stream includes a sucralose-6-acylate, the reaction vehicle, water, and salts. The salts include one or more selected from the group consisting of alkali metal chlorides, alkaline earth metal chlorides and ammonium chloride. The method includes: (i) deacylation of the sucralose-6-acylate by treatment with a base to afford a product stream comprising sucralose; (ii) partial removal of water and, optionally, reaction vehicle from the product stream of (i) in order to cause precipitation of the salts from the product stream; (iii) removal of the precipitated salts from the product stream of (ii); and (iv) isolation of sucralose from the product stream of (iii).
摘要翻译：本发明提供了由反应载体中蔗糖-6-酰化物的氯化得到的进料流中生产三氯蔗糖的方法。进料流包括三氯蔗糖-6-酰化物，反应载体，水和盐。所述盐包括选自碱金属氯化物，碱土金属氯化物和氯化铵中的一种或多种。该方法包括：（i）用碱处理三氯半乳蔗糖-6-酰化物脱酰基，得到包含三氯蔗糖的产物流; （ii）从（i）的产物流中部分除去水和任选的反应载体，以便使产物流中的盐沉淀; （iii）从（ii）的产物流中除去沉淀的盐; 和（iv）从（iii）的产物流中分离三氯半乳蔗糖。

4. 发明申请

US20090299055A1 Purification of Sucralose Containing Feed Streams for Sucralose Crystallization 审中-公开
标题翻译：含三氯蔗糖的三氯蔗糖结晶原料的纯化
公开(公告)号：US20090299055A1
公开(公告)日：2009-12-03
申请号：US12412832
申请日：2009-03-27
申请人： James Edwin Wiley, JR. , John Kerr , Robert Jansen , Gordon Walker
发明人： James Edwin Wiley, JR. , John Kerr , Robert Jansen , Gordon Walker
IPC分类号： C07H1/06
CPC分类号： C07H1/06 , C07H5/02
摘要： A process for the recovery of a carbohydrate selected from sucralose and sucralose-6-esters from an aqueous feed stream is disclosed. The process comprises extracting the feed stream with an organic solvent, such as ethyl acetate, back extracting the resulting carbohydrate-containing organic extract with an aqueous solvent, and either crystallizing the carbohydrate from the organic solvent or replacing the organic solvent with water and crystallizing the carbohydrate from water. The process results in an increased overall yield of the carbohydrate.
摘要翻译：公开了从含水进料流中回收选自三氯蔗糖和三氯蔗糖-6-酯的碳水化合物的方法。该方法包括用有机溶剂如乙酸乙酯萃取进料流，用水溶剂反萃取所得含碳水化合物的有机萃取物，并将碳水化合物从有机溶剂中结晶或用水代替有机溶剂，并使来自水的碳水化合物该方法导致碳水化合物的总收率提高。

5. 发明申请

US20090281295A1 CRYSTALLIZATION OF SUCRALOSE FROM SUCRALOSE-CONTAINING FEED STREAMS 审中-公开
标题翻译：含有包含进料流的SUCRALOSE的结晶
公开(公告)号：US20090281295A1
公开(公告)日：2009-11-12
申请号：US12417153
申请日：2009-04-02
申请人： Edward Micinski , James Edwin Wiley, JR. , Duane A. Leinhos , Mark R. Huber
发明人： Edward Micinski , James Edwin Wiley, JR. , Duane A. Leinhos , Mark R. Huber
IPC分类号： C07H17/04
CPC分类号： C07H5/02 , C07H1/06
摘要： A process for the purification of sucralose in sucralose-containing feed streams is disclosed. The process includes multiple liquid-liquid extraction steps; optionally, a concentration step; multiple crystallization steps; optionally, a chromatography step; and various recycle steps.
摘要翻译：公开了一种在含三氯蔗糖的进料流中纯化三氯蔗糖的方法。该方法包括多个液 - 液萃取步骤; 任选地，浓缩步骤; 多结晶步骤; 任选地，色谱步骤; 和各种回收步骤。

6. 发明申请

US20090259036A1 EXTRACTION OF LESS POLAR IMPURITIES FROM SUCRALOSE CONTAINING AQUEOUS FEED STREAMS 审中-公开
标题翻译：从含有水分的饲料中提取较少的极性污染物
公开(公告)号：US20090259036A1
公开(公告)日：2009-10-15
申请号：US12416541
申请日：2009-04-01
申请人： James Edwin Wiley, JR.
发明人： James Edwin Wiley, JR.
IPC分类号： C07H1/06
CPC分类号： C07H5/02
摘要： A process for the purification of sucralose containing aqueous feed streams is disclosed. The process comprises the step of extracting an aqueous feed stream comprising sucralose and impurities less polar than sucralose, such as tetrachloro saccharides, with an organic solvent that is immiscible with water, such as ethyl acetate. In this step, the mass ratio of organic solvent to aqueous feed stream is in the range of 0.4 to 0.9. Greater than 50% of the sucralose and greater than 95% of the tetrachloro saccharide impurities are extracted into the organic extract. The organic extract is back extracted with water and the resulting aqueous extract recycled to the initial extraction step.
摘要翻译：公开了一种用于纯化含三氯蔗糖含水进料流的方法。该方法包括提取包含三氯半乳蔗糖和比三氯半乳蔗糖（例如四氯糖）极性少的杂质的水性进料流与与水不混溶的有机溶剂，例如乙酸乙酯。在该步骤中，有机溶剂与水性进料流的质量比在0.4至0.9的范围内。将大于50％的三氯蔗糖和大于95％的四氯糖杂质提取到有机提取物中。将有机萃取液用水反萃取，将所得含水萃取液再循环至初始萃取步骤。

7. 发明申请

US20120289693A1 Extraction of Carboxylic Acids with Tin Compounds 有权
标题翻译：用锡化合物萃取羧酸
公开(公告)号：US20120289693A1
公开(公告)日：2012-11-15
申请号：US13463332
申请日：2012-05-03
申请人： David T. Coleman , Edward Micinski , James Edwin Wiley, JR. , Thomas A. Eilers , David A. Dentel
发明人： David T. Coleman , Edward Micinski , James Edwin Wiley, JR. , Thomas A. Eilers , David A. Dentel
IPC分类号： C07C231/24 , C07H1/06 , C07H1/00
CPC分类号： B01D11/04 , C07H13/02
摘要： A method of removing a carboxylic acid from a liquid including a tertiary amide solvent includes: A) forming an extraction medium including an acid-extracting tin species and an extraction solvent that is immiscible with the tertiary amide solvent; B) subsequently contacting the liquid with the extraction medium, forming a phase including a de-acidified tertiary amide solvent and a phase including the extraction solvent; and C) removing the phase including the extraction solvent, to afford a liquid including the de-acidified tertiary amide solvent. The acid-extracting tin species is one or more tin species obtainable by reaction of a di(hydrocarbyl)tin oxide with less than one equivalent of a carboxylic acid, tin species obtainable by reaction of a 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl)distannoxane with an aqueous base. A method of preparing a sucralose-6-acylate includes using the foregoing method to remove a carboxylic acid from a liquid including a tertiary amide solvent and the sucralose-6-acylate.
摘要翻译：从包括叔酰胺溶剂的液体中除去羧酸的方法包括：A）形成包含酸提取锡物质的萃取介质和与叔酰胺溶剂不混溶的萃取溶剂; B）随后使液体与提取介质接触，形成包含脱酸叔胺溶剂和包含萃取溶剂的相的相; 和C）除去包括萃取溶剂的相，得到包含脱酸叔酰胺溶剂的液体。酸提取锡物质是通过二（烃基）氧化锡与小于1当量羧酸反应获得的一种或多种锡物质，可通过1,3-二酰氧基-1,1， 3,3-四（烃基）二锡氧烷与碱水溶液。制备三氯蔗糖-6-酰化物的方法包括使用上述方法从包括叔酰胺溶剂和三氯蔗糖-6-酰化物的液体中除去羧酸。

8. 发明授权

US08212022B2 Effect of carbohydrate concentration on sucralose extraction efficiency 有权
标题翻译：碳水化合物浓度对三氯蔗糖提取效率的影响
公开(公告)号：US08212022B2
公开(公告)日：2012-07-03
申请号：US12416520
申请日：2009-04-01
申请人： Edward Micinski , James Edwin Wiley, Jr.
发明人： Edward Micinski , James Edwin Wiley, Jr.
IPC分类号： C07H1/06
CPC分类号： C07H1/06 , C07H5/02
摘要： A process for the purification of aqueous feed streams containing sucralose and/or sucralose 6-esters includes, providing an aqueous feed stream including the sucralose and/or sucralose 6-esters, concentrating the aqueous feed stream to form a concentrated aqueous feed stream containing at least 10 wt % total carbohydrates and extracting the concentrated aqueous feed stream with an organic solvent and producing an organic extract and an aqueous extract, in which the organic solvent is immiscible with water, and in which the carbohydrate preferentially passes into the organic extract.
摘要翻译：用于纯化含有三氯蔗糖和/或三氯蔗糖-6-酯的含水进料流的方法包括提供包含三氯半乳蔗糖和/或三氯蔗糖6-酯的含水进料流，浓缩含水进料流以形成含有至少10重量％的总碳水化合物，并用有机溶剂萃取浓缩的含水进料流，并产生有机萃取物和水提取物，其中有机溶剂与水不混溶，并且其中碳水化合物优先进入有机萃取物。

9. 发明申请

US20120157675A1 PURIFICATION OF TERTIARY FORMAMIDE CONTAMINATED WITH TERTIARY ACETAMIDE 有权
标题翻译：纯化用苛性乙酰胺污染的腐殖酸
公开(公告)号：US20120157675A1
公开(公告)日：2012-06-21
申请号：US13378531
申请日：2010-06-18
申请人： James Edwin Wiley, JR. , Mohamad R. Jaber
发明人： James Edwin Wiley, JR. , Mohamad R. Jaber
IPC分类号： C07H5/02 , C07C233/03
CPC分类号： C07C231/24 , C07H1/06 , C07H5/02 , C07C233/03
摘要： A chlorinating agent such as a chloroiminium species is used to remove or neutralize tertiary acetamide present as a contaminant in a tertiary formamide solvent. Tertiary formamide solvent purified or treated in this manner can be used as a reaction vehicle for the chlorination of sucrose-6-acylates, thereby improving the yields of the desired sucralose-6-acylate (an intermediate in the production of sucralose).
摘要翻译：使用氯化剂如氯亚胺鎓物质来除去或中和作为叔甲酰胺溶剂中的污染物存在的叔乙酰胺。以这种方式纯化或处理的叔甲酰胺溶剂可用作蔗糖-6-酰化物氯化反应载体，从而提高所需三氯半乳蔗糖-6-酰化物（三氯蔗糖生产中的中间体）的产率。

10. 发明申请

US20110087018A1 Low Temperature, Single Solvent Process for the Production of Sucrose-6-Ester 有权
标题翻译：用于生产蔗糖-6-酯的低温单溶剂方法
公开(公告)号：US20110087018A1
公开(公告)日：2011-04-14
申请号：US12901808
申请日：2010-10-11
申请人： Edward Micinski , David Coleman , James Edwin Wiley, JR.
发明人： Edward Micinski , David Coleman , James Edwin Wiley, JR.
IPC分类号： C07H1/00
CPC分类号： C07H13/04 , C07F7/2224 , C07H13/06 , C07H13/08
摘要： A method for the preparation of a sucrose-6-ester is disclosed. In a first step of the method, sucrose in a polar aprotic solvent is reacted with an organotin-based acylation promoter. The water of reaction is removed at a temperature that does not exceed about 80° C. In one aspect, the water is removed by distillation of part of the polar aprotic solvent at reduced pressure. In a second step, a carboxylic acid anhydride is added. In one aspect, the resulting reaction mixture is maintained at a temperature of 10° C. or less for a period of time sufficient to produce a sucrose-6-ester. The sucrose-6-ester can be converted to sucralose.
摘要翻译：公开了制备蔗糖-6-酯的方法。在该方法的第一步中，将极性非质子溶剂中的蔗糖与基于有机锡的酰化促进剂反应。在不超过约80℃的温度下除去反应水。在一个方面，通过在减压下蒸馏部分极性非质子溶剂除去水。在第二步中，加入羧酸酐。一方面，所得反应混合物在10℃或更低的温度下保持足以产生蔗糖-6-酯的时间。蔗糖-6-酯可以转化成三氯蔗糖。

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