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公开(公告)号：US07049435B2
公开(公告)日：2006-05-23
申请号：US10092715
申请日：2002-03-08
申请人： Steven J. Catani , Nicholas M. Vernon , David Saul Neiditch , James Edwin Wiley, Jr. , Edward Micinski
发明人： Steven J. Catani , Nicholas M. Vernon , David Saul Neiditch , James Edwin Wiley, Jr. , Edward Micinski
IPC分类号： C07H1/06
摘要： The present invention relates to novel extractive methods for purifying sucralose. The present invention also relates to compositions comprising the sucralose preparations made by the methods of the present invention.
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公开(公告)号：US06998480B2
公开(公告)日：2006-02-14
申请号：US10092730
申请日：2002-03-08
IPC分类号： C07H13/02
摘要： This invention relates to processes for purifying sucralose by the use of an initial non-crystallization purification procedure followed by three or more sequential crystallization steps and recycle of the mother liquor remaining from each crystallization step to the feed of another crystallization or purification step. This invention also relates to sucralose compositions as well as compositions comprising the sucralose compositions of the present invention. These compositions may be highly pure and have a superior taste profile.
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公开(公告)号：US06890581B2
公开(公告)日：2005-05-10
申请号：US10116758
申请日：2002-04-05
摘要： The present invention relates to novel methods for stabilizing aqueous deacylation, via use of buffers in the production of sucralose. The present invention provides a process for producing sucralose from an acyl-sucralose compound whereby the acyl-sucralose compound is deacylated in the presence of a buffering agent, which stabilizes the pH of the feed mixture and decreases the accumulation of undesired anhydro compounds. Further, the present invention provides a process whereby the acyl-sucralose compound is deacylated directly either prior to or after removal of the tertiary amide reaction vehicle from the neutralized chlorination feed mixture. An aqueous solution of sucralose including salts and other compounds is produced, from which sucralose is recovered by extraction and purified by crystallization.
摘要翻译： 本发明涉及通过在制备三氯蔗糖中使用缓冲液来稳定水解性脱酰基的新方法。 本发明提供了由酰基 - 三氯蔗糖化合物制备三氯半乳蔗糖的方法，其中酰基 - 三氯蔗糖化合物在缓冲剂存在下脱酰基化，其稳定了进料混合物的pH并降低了不期望的脱水化合物的积累。 此外，本发明提供了一种方法，其中酰基 - 三氯蔗糖化合物在从中和的氯化进料混合物中除去叔酰胺反应介质之前或之后直接脱酰基化。 产生包括盐和其它化合物的三氯半乳蔗糖水溶液，通过萃取回收三氯蔗糖并通过结晶纯化。
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公开(公告)号：US06943248B2
公开(公告)日：2005-09-13
申请号：US10426387
申请日：2003-04-30
摘要： A crystalline form of sucralose, and a method of making it. The method involves continuously crystallizing sucralose from an aqueous solution by a process providing continuous removal and recirculation of the vessel contents, and providing a long residence time for sucralose in the system. The crystals thus formed are of a relatively low length/diameter ratio, have an unsymmetrical shape, and exhibit good stability. The larger crystals in particular are tapered as compared to the rod-like larger crystals in prior art product.
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5.发明授权Process for recovery of organotin esters from reaction mixtures containing the same and re-use of the recovered organotin compounds 失效从含有该有机锡酯的反应混合物中回收有机锡酯的方法，并重新利用回收的有机锡化合物
公开(公告)号：US5034551A
公开(公告)日：1991-07-23
申请号：US512690
申请日：1990-04-23
CPC分类号： C07H13/04 , C07F7/2256 , C07H13/08
摘要： A process which comprises extracting 1,3-diacyloxy-1,1,3,3-tetra(hydrocarbyl) distannoxane from a mixture containing 1,3-diacyloxy-1,1,3,3-tetra(hydrocarbyl)distannoxane, a sucrose-6-ester, and polar aprotic solvent, which process comprises the steps of:(a) contacting said mixture, in the presence of a small amount of water, with an organic solvent that is substantially immiscible with water to form thereby an extraction mixture, wherein the amount of water employed is sufficient to cause efficient partitioning of said 1,3-diacyloxy-1,1,3,3-tetra(hydrocarbyl)distannoxane from a first phase comprising said polar aprotic solvent into second phase comprising said organic solvent;(b) agitating the extraction mixture for a period of time and at a temperature sufficient to form thereby a two-phase mixture wherein the preponderance of the 1,3-diacyloxy-1,1,3,3-tetra(hydrocabyl)distannoxane in the extraction mixture is contained in said second phase and essentially all of the sucrose-6-ester in the extraction mixture is contained in said first phase; and(c) separating said first phase from said second phase.
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公开(公告)号：US4980463A
公开(公告)日：1990-12-25
申请号：US382147
申请日：1989-07-18
CPC分类号： C07H5/02
摘要： A process for the chlorination of sucrose-6-esters to produce 6',4,1'-trichlorosucrose-6-esters which comprises the steps of:(a) adding at least seven molar equivalents of an acid chloride to a reaction mixture containing a sucrose-6-ester and a tertiary amide to form initially a chloroformiminium chloride salt which subsequently forms a complex with the hydroxyl groups of the sucrose-6-ester;(b) subjecting the reaction mixture product of step (a) to an elevated temperature not higher than about 85.degree. C. for a period of time sufficient to produce a mixture of chlorinated sucrose-6-ester products consisting essentially of 6'-chlorosucrose-6-ester, 4,6'-dichlorosucrose-6-ester, and 1',6'-dichlorosucrose-6-ester; and(c) subjecting the reaction mixture product of step (b) to an elevated temperature not higher than about 125.degree. C. for a period of time sufficient to produce a chlorinated product consisting essentially of 1',4,6'-trichlorosucrose-6-ester.
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公开(公告)号：US5136031A
公开(公告)日：1992-08-04
申请号：US474314
申请日：1990-07-09
摘要： A process for the chlorination of sucrose or a derivative thereof, comprises reaction of the sucrose or derivative thereof with thionyl chloride and a nitrogen base at a ratio of about 1 molar equivalent (ME) of thionyl chloride and about 1 ME of base for every ME of free hydroxyl, in a non-reactive moderately polar solvent. The process is particularly suitable for the preparation of sucralose.
摘要翻译： 蔗糖或其衍生物的氯化方法包括将蔗糖或其衍生物与亚硫酰氯和氮碱按每摩尔约1摩尔当量（ME）亚硫酰氯和约1ME碱的比例反应 的游离羟基，在非反应性中等极性溶剂中。 该方法特别适用于制备三氯蔗糖。
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公开(公告)号：US5023329A
公开(公告)日：1991-06-11
申请号：US512692
申请日：1990-04-23
摘要： Process which comprises reacting sucrose with a di-(hydrocarbyl)tin oxide in an inert organic reaction vehicle with removal of water for a period of time and at a temperature sufficient to produce a 1,3-di-(6-O-sucrose)-1,1,3,3-tetra(hydrocarbyl)distannoxane.
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公开(公告)号：US5470969A
公开(公告)日：1995-11-28
申请号：US237947
申请日：1994-05-02
摘要： Sucrose is mono-acylated in the 6-position by reacting sucrose with a carboxylic acid anhydride such as acetic or benzoic anhydride in a reaction mixture containing a polar aprotic solvent and a catalytic quantity of a 1,3-diacyloxy-1,1,3,3-tetra(hydrocarbyl)distannoxane, for a period of time and at a temperature sufficient to produce a sucrose-6-ester.
摘要翻译： 蔗糖通过蔗糖与羧酸酐如乙酸或苯甲酸酐在含有极性非质子溶剂和催化量的1,3-二酰氧基-1,1,3,3-四氢呋喃的反应混合物中在6-位上单酰化 ，3-四（烃基）二锡氧烷，持续一段时间并在足以产生蔗糖-6-酯的温度下进行。
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10.发明授权Process for the preparation of 1,6-dichloro-1,6-dideoxy-.beta.-D-fructofuranosyl-4-chloro-4-deoxy-.alpha. - 失效制备1,6-二氯-1,6-二脱氧-β-D-呋喃果糖基-4-氯-4-脱氧-α-吡喃半乳糖苷的方法
公开(公告)号：US4801700A
公开(公告)日：1989-01-31
申请号：US921285
申请日：1986-10-20
摘要： A process for the preparation of 1,6-dichloro-1,6-dideoxy-.beta.-D-fructofuranosyl-4-chloro-4-deoxy-.alpha.-galactopyranoside comprising the steps of (a) reacting sucrose with a tritylating agent; (b) acetylating the tritylated reaction product; (c) detritylating the acetylated reaction product; (d) isomerizing the resulting penta-acetate; (e) chlorinating the isomerized product; and (f) deacetylating the chlorinated reaction product.
摘要翻译： 制备1,6-二氯-1,6-二脱氧-β-D-呋喃果糖基-4-氯-4-脱氧-α-吡喃半乳糖苷的方法，包括以下步骤：（a）使蔗糖与三苯甲基化试剂反应; （b）三苯甲基化反应产物乙酰化; （c）使乙酰化反应产物脱铁; （d）使所得五乙酸异构化; （e）氯化异构化产物; 和（f）使氯化反应产物脱乙酰化。
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