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公开(公告)号：US08796446B2
公开(公告)日：2014-08-05
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： C07H1/06 , C07H1/00 , C07C231/24
摘要： A method of removing a carboxylic acid from a liquid including a tertiary amide solvent includes: forming an extraction medium including an acid-extracting tin species and an extraction solvent that is immiscible with the tertiary amide solvent; 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 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 obtained by reaction of a di(hydrocarbyl) tin oxide with less than one equivalent of a carboxylic acid, or 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 uses 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：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; 随后使液体与提取介质接触，形成包含脱酸叔酰胺溶剂和包含萃取溶剂的相的相; 并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当量羧酸的反应获得的一种或多种锡物质，或通过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。
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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
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。
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公开(公告)号：US08436157B2
公开(公告)日：2013-05-07
申请号：US12409951
申请日：2009-03-24
IPC分类号： 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。
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公开(公告)号：US20090247737A1
公开(公告)日：2009-10-01
申请号：US12409951
申请日：2009-03-24
IPC分类号： 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。
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公开(公告)号：US20120077972A1
公开(公告)日：2012-03-29
申请号：US13260441
申请日：2010-03-24
IPC分类号： C08B37/00
摘要： A method for the chlorination of a sucrose-6-acylate to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-β-acylate wherein said method comprises: (i) reacting the sucrose-6-acylate with a chlorinating agent in a reaction vehicle comprising a tertiary amide in order to chlorinate the 4, V and 6′ positions of the sucrose-6-acylate; and (ii) quenching the product stream of (i) to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate; wherein before said quenching, a portion of the tertiary amide is removed.
摘要翻译： 用于氯化蔗糖-6-酰化物以产生4,1'，6'-三氯-4,1'，6'-三脱氧 - 半乳糖蔗糖 - 乙酸酯的方法，其中所述方法包括：（i）使 蔗糖-6-酰化物与含有叔酰胺的反应载体中的氯化剂以将蔗糖-6-酰化物的4，V和6'位置氯化; （ii）淬灭（i）的产物流以产生4,1'，6'-三氯-4,1'，6'-三脱氧 - 半乳糖蔗糖-6-酰化物; 在所述淬火之前，一部分叔酰胺被除去。
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公开(公告)号：US08530643B2
公开(公告)日：2013-09-10
申请号：US13260441
申请日：2010-03-24
摘要： A method for the chlorination of a sucrose-6-acylate to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-β-acylate wherein said method comprises: (i) reacting the sucrose-6-acylate with a chlorinating agent in a reaction vehicle comprising a tertiary amide in order to chlorinate the 4, V and 6′ positions of the sucrose-6-acylate; and (ii) quenching the product stream of (i) to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate; wherein before said quenching, a portion of the tertiary amide is removed.
摘要翻译： 蔗糖-6-酰化物氯化以产生4,1'，6'-三氯-4,1'，6'-三脱氧 - 半乳糖蔗糖-β-酰化物的方法，其中所述方法包括：（i）使 蔗糖-6-酰化物与含有叔酰胺的反应载体中的氯化剂以将蔗糖-6-酰化物的4，V和6'位置氯化; （ii）淬灭（i）的产物流以产生4,1'，6'-三氯-4,1'，6'-三脱氧 - 半乳糖蔗糖-6-酰化物; 在所述淬火之前，一部分叔酰胺被除去。
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公开(公告)号：US20080227971A1
公开(公告)日：2008-09-18
申请号：US12004260
申请日：2007-12-20
IPC分类号： C07H1/06
CPC分类号： C07H5/02
摘要： A method of making sucralose includes maintaining a solution of a sucralose-6-acylate in an aqueous solvent at a temperature in a range from −20° C. to 20° C. and at a pH of at least 12.2 and less than 14.0 for a period of time sufficient to deacylate substantially all of the sucralose-6-acylate. The method may employ purified sucralose-6-acylate as the starting material, or the sucralose-6-acylate may be present in a quenched reaction mixture resulting from chlorination of a sucrose-6-acylate. The quenched reaction mixture may be exposed to deacylation conditions either before or after removal of a tertiary amide that may be present in it. Sucralose is subsequently recovered to complete the process.
摘要翻译： 制备三氯蔗糖的方法包括在-20℃至20℃的温度范围内保持三氯蔗糖-6-酰化物在水性溶剂中的溶液，并且在至少12.2和小于14.0的pH下保持 足以使基本上所有的三氯蔗糖-6-酰化物脱酰基化的时间。 该方法可以使用纯化的三氯半乳蔗糖-6-酰化物作为起始原料，或三氯蔗糖-6-酰化物可存在于由蔗糖-6-酰化物氯化得到的骤冷反应混合物中。 在除去可能存在的叔酰胺之前或之后，骤冷的反应混合物可能暴露于脱酰基化条件。 随后回收三氯蔗糖以完成该过程。
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公开(公告)号：US4349488A
公开(公告)日：1982-09-14
申请号：US317613
申请日：1981-11-03
申请人： David A. Dentel , David C. Sanders
发明人： David A. Dentel , David C. Sanders
IPC分类号： C07C20060101 , C07C255/38 , C07C255/49 , C07C255/53 , C07C121/75
CPC分类号： C07C255/00 , Y02P20/584
摘要： 2,6-dibromo-4-cyanophenyl octanoates and other esters of 3,5-dibromo-4-hydroxybenzonitrile may be produced by reacting 4-hydroxybenzonitrile with bromine in the presence of an inert solvent and catalytic amounts of a basic heterocyclic aromatic compound or its hydrohalide, followed by removal of unreacted bromine and addition of octanoyl chloride or other acyl halide to the reaction mixture and recovery of the desired ester together with recyclable pyridine hydrohalide catalyst and solvent.
摘要翻译： 2,6-二溴-4-氰基苯基辛酸酯和3,5-二溴-4-羟基苄腈的其它酯可以通过4-羟基苄腈与溴在惰性溶剂和催化量的碱性杂环芳族化合物的存在下反应来制备，或 然后除去未反应的溴，并向反应混合物中加入辛酰氯或其它酰基卤，并与可回收的吡啶氢卤酸酯催化剂和溶剂一起回收所需的酯。
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