Chlorination of sucrose-6-esters
    1.
    发明授权

    公开(公告)号:US10081651B2

    公开(公告)日:2018-09-25

    申请号:US15502372

    申请日:2015-06-16

    IPC分类号: C07H5/02 C07H13/04

    CPC分类号: C07H5/02 C07H13/04

    摘要: There is provided a method for the chlorination of a sucrose-6-acylate to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate, wherein said method comprises the following steps (i) to (v): (i) providing a first component comprising sucrose-6-acylate; (ii) providing a second component comprising a chlorinating agent; (iii) combining said first component and said second component to afford a mixture; (iv) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4, 1′ and 6′ positions thereof; (v) quenching said mixture to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate; wherein at least one of said first component and said second component comprises a reaction vehicle, and said reaction vehicle comprises a tertiary amide; and wherein said mixture comprises a cosolvent during a least a portion of the heating period of step (iv), wherein said cosolvent comprises dimethylacetamide (DMAc).

    Purification of tertiary formamide contaminated with tertiary acetamide
    3.
    发明授权
    Purification of tertiary formamide contaminated with tertiary acetamide 有权
    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

    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。

    Chlorination of sucrose-6-esters
    4.
    发明授权

    公开(公告)号:US10227367B2

    公开(公告)日:2019-03-12

    申请号:US15104620

    申请日:2014-12-15

    摘要: There is provided a method for the chlorination of a sucrose-6-acylate to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate, wherein said method comprises the following steps (i) to (v): (i) providing a first component comprising sucrose-6-acylate; (ii) providing a second component comprising a chlorinating agent; (iii) combining said first component and said second component to afford a mixture; (iv) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4, 1′ and 6′ positions thereof; (v) quenching said mixture to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate; wherein at least one of said first component and said second component comprises a reaction vehicle, and said reaction vehicle comprises a tertiary amide; and wherein said mixture comprises a cosolvent during a least a portion of the heating period of step (iv), wherein said cosolvent comprises perfluorooctane.

    Extraction of Carboxylic Acids with Tin Compounds
    6.
    发明申请
    Extraction of Carboxylic Acids with Tin Compounds 有权
    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

    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。

    Effect of carbohydrate concentration on sucralose extraction efficiency
    7.
    发明授权
    Effect of carbohydrate concentration on sucralose extraction efficiency 有权
    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

    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。

    PURIFICATION OF TERTIARY FORMAMIDE CONTAMINATED WITH TERTIARY ACETAMIDE
    8.
    发明申请
    PURIFICATION OF TERTIARY FORMAMIDE CONTAMINATED WITH TERTIARY ACETAMIDE 有权
    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

    IPC分类号: 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。

    Molten Salt Treatment System and Process
    9.
    发明申请
    Molten Salt Treatment System and Process 审中-公开
    熔盐处理系统和工艺

    公开(公告)号:US20110294083A1

    公开(公告)日:2011-12-01

    申请号:US13142555

    申请日:2009-12-29

    IPC分类号: F24J3/00 B01J19/00

    摘要: A molten salt treatment system and process can include one or more tubular conduits flowably connected to a molten salt reactor, the tubular conduit containing concentrically within it a pipe or a shaft separated by an annular space therebetween, and one or more gas sources connected to feed gas into the annular space. The system may include a scrubbing device flowably connected to a molten salt reactor off-gas outlet to receive an off-gas, a first heating device configured to heat the effluent from the scrubbing device, and a filtering device flowably connected to receive the effluent from the heating device. An overflow conduit may be flowably connected to a molten salt reactor overflow outlet to receive molten salt therefrom and discharge the molten salt to a salt recovery vessel, and a blower or other gas mover may be connected to the molten salt reactor and the recovery vessel to prevent backflow of cold gases through the overflow outlet to the molten salt reactor.

    摘要翻译: 熔盐处理系统和过程可以包括一个或多个可流动地连接到熔盐反应器的管状导管,管状导管同心地包含一个管或由它们之间的环形空间隔开的轴,以及连接到进料的一个或多个气源 气体进入环形空间。 该系统可以包括可流动地连接到熔盐反应器废气出口以接收废气的洗涤装置,被配置为加热来自洗涤装置的流出物的第一加热装置和可流动地连接以接收来自 加热装置。 溢流导管可以可流动地连接到熔盐反应器溢流出口,以从其中接收熔融盐,并将熔融盐排出到盐回收容器中,并且鼓风机或其它气体移动器可以连接到熔盐反应器和回收容器 防止冷气体通过溢流出口回流到熔盐反应器。

    Low Temperature, Single Solvent Process for the Production of Sucrose-6-Ester
    10.
    发明申请
    Low Temperature, Single Solvent Process for the Production of Sucrose-6-Ester 有权
    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

    IPC分类号: C07H1/00

    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。