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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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公开(公告)号：US5298611A
公开(公告)日：1994-03-29
申请号：US30518
申请日：1993-03-12
摘要： A process for producing substantially pure sucralose pentaester from a mixture of 6-O-acyl-4,1' ,6' -trichloro-4,1',6'-trideoxygalactosucrose in a reaction medium comprising a tertiary amide, wherein said process comprises the steps of:(a) recovering the 6-O-acyl-4,1' ,6' -trichloro-4,1' ,6' -trideoxygalactosucrose from said mixture;(b) peracylating the 6-O-acyl-4,1' ,6' -trichloro-4,1' ,6' -trideoxygalactosucrose product of step (a) to produce thereby 4,1',6' -trichloro-4,1' ,6' -trideoxygalactosucrose pentaester; and(c) crystallizing the 4,1',6' -trichloro-4,1' ,6' -trideoxygalactosucrose pentaester product of step (b) to produce substantially pure 4,1',6' -trichloro-4,1' ,6' -trideoxygalactosucrose pentaester.
摘要翻译： 一种从含有叔酰胺的反应介质中由6-O-酰基-4,1'，6'-三氯-4,1'，6'-三脱氧半乳蔗糖的混合物制备基本上纯的三氯蔗糖五酯的方法，其中所述方法包括 步骤：（a）从所述混合物中回收6-O-酰基-4,1'，6'-三氯-4,1'，6'-三脱氧半乳糖蔗糖; （b）使步骤（a）的6-O-酰基-4,1'，6'-三氯-4,1'，6'-三脱氧半乳糖蔗糖酯过酰化从而产生4,1'，6'-三氯-4 ，1'，6'-三脱氧半乳蔗糖五酯; 和（c）使步骤（b）的4,1'，6'-三氯-4,1'，6'-三脱氧半乳糖蔗糖五酯产物结晶以产生基本上纯的4,1'，6'-三氯-4,1' 6'-三脱氧半乳蔗糖五酯。
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4.发明授权Selective 6-acylation of sucrose mediated by cyclic adducts of dialkyltin oxides and diols 失效二环烷基氧化物和二醇的循环添加引起的蔗糖的选择性6-取代
公开(公告)号：US5089608A
公开(公告)日：1992-02-18
申请号：US499731
申请日：1990-03-23
CPC分类号： C07H13/04 , C07F7/2232 , C07H13/06 , C07H13/08 , C07H23/00
摘要： There is disclosed a process which comprises the steps of:(a) reacting a di(hydrocarbyl)tin oxide such as a dialkyltin oxide with a dihydric alcohol, alkanolamine, or an enolizable .alpha.-hydroxyketone in an inert organic reaction vehicle, with removal of water, at a temperature and for a period of time sufficient to produce a cyclic adduct of said dialkyltin oxide and said dihydric alcohol, alkanolamine, or enolizable .alpha.-hydroxyketone;(b) reacting said cyclic adduct product of Step (a) with sucrose in an inert organic reaction vehicle such as a dipolar aprotic liquid, at a temperature and for a period of time sufficient to produce a 6-O-[dihydrocarbyl(hydroxy- or amino- or oxohydrocarbyl)stannoxyl]sucrose; and(c) reacting the product of Step (b) with an acylating agent to produce a sucrose-6-ester.
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5.发明授权Production of sucralose without intermediate isolation of crystalline sucralose-6-ester 失效生产三氯半乳蔗糖而不中间分离结晶三氯半乳蔗糖-6-酯
公开(公告)号：US5498709A
公开(公告)日：1996-03-12
申请号：US448710
申请日：1995-05-24
CPC分类号： C07H5/02
摘要： There is disclosed a process for producing sucralose from sucralose-6-ester whereby the sucralose-6-ester is deacylated directly either prior to or after removal of the tertiary amide reaction vehicle from the neutralized chlorination reaction mixture, to produce an aqueous solution of sucralose plus salts and impurities, from which sucralose is recovered by extraction and is then preferably purified by crystallization.
摘要翻译： 公开了一种由三氯蔗糖-6-酯制备三氯半乳蔗糖的方法，由此三氯蔗糖-6-酯在从中和的氯化反应混合物中除去叔胺反应载体之前或之后直接脱酰基，以产生三氯半乳蔗糖的水溶液 加上盐和杂质，通过萃取从其中回收三氯蔗糖，然后优选通过结晶纯化。
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6.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：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：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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