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11. 发明申请

US20100160625A1 Novel Preparation of 6-O-Acyl Chlorosucrose from Anhydrous Cholorinated Reaction Mass 审中-公开
标题翻译：从无水氯化反应物质中新制备6-O-酰基氯蔗糖
公开(公告)号：US20100160625A1
公开(公告)日：2010-06-24
申请号：US11992431
申请日：2006-09-21
申请人： Rakesh Ratnam , Sundeep Aurora , Srikanth Kulkarni
发明人： Rakesh Ratnam , Sundeep Aurora , Srikanth Kulkarni
IPC分类号： C07H1/08
CPC分类号： C07H1/06 , C07H3/04 , C07H5/02
摘要： A process is described for production of a chlorinated sucrose from a process stream containing a 6-O-protected chlorinated sucrose derived from chlorination of 6-O-protected sucrose wherein the process stream is treated under conditions which prevent or reverse deacylation of 6-O-protected chlorinated sucrose, extracting the same in a solvent, washing most of the dimethylformamide free from the solvent extract by repeated washing with saturated sodium chloride solution, isolating the 6-O-protected sucrose as a pure fraction and obtaining a chlorinated sucrose by deacylating the same.
摘要翻译：描述了从含有6-O-保护的蔗糖氯化的6-O保护的氯化蔗糖的工艺流中生产氯化蔗糖的方法，其中将工艺流在防止或逆转6-O保护的蔗糖的脱酰基的条件下处理保护的氯化蔗糖，在溶剂中萃取相同的溶剂，通过用饱和氯化钠溶液反复洗涤将大部分无溶剂的二甲基甲酰胺溶解在溶剂提取物中，分离出6-O保护的蔗糖为纯级分，通过去酰基化得到氯化蔗糖一样。

12. 发明申请

US20090208747A1 Novel Crystalline Methods and Novel Crystalline and Amorphous forms of Halogenated Sugars 审中-公开
标题翻译：新型结晶方法和新型结晶和无定形形式的卤代糖
公开(公告)号：US20090208747A1
公开(公告)日：2009-08-20
申请号：US12225378
申请日：2007-03-21
申请人： Rakesh Ratnam , Chandrashekar Batchu , Andanagouda Patil , Sundeep Aurora
发明人： Rakesh Ratnam , Chandrashekar Batchu , Andanagouda Patil , Sundeep Aurora
IPC分类号： C13K13/00 , B32B5/16
CPC分类号： C07H5/02 , C07H1/00 , Y10T428/2982
摘要： Disclosed is crystalline 4,1′,6′Trichlorogalactosucrose (TGS) having enhanced storage stability, a mean particle size of about 5 microns or less, 90% particles being less than about 10 microns and the maximum particle size being more than twice the mean but less than about 35 microns; and a process for producing the same comprising gradual cooling of a saturated solution of TGS of a mixture of a a polar alcoholic solvent and a less polar organic solvent, the proportion of the said polar alcoholic solvent being within maintained within a range of about 3% to 10% of total volume of the said saturated solution during cooling process.
摘要翻译：公开了具有增强的储存稳定性，平均粒度约5微米或更小的结晶4,1'，6'-三氯半乳糖（TGS），90％颗粒小于约10微米，最大颗粒大小是平均值的两倍但小于约35微米; 以及其制备方法，包括逐渐冷却极性醇溶剂和极性较小的有机溶剂的混合物的TGS的饱和溶液，所述极性醇溶剂的比例在约3％的范围内保持在在冷却过程中所述饱和溶液的总体积的10％。

13. 发明申请

US20090105470A1 Tin Mediated Regioselective Synthesis of Sucrose-6-Esters 审中-公开
标题翻译：锡介导的区域选择性合成蔗糖-6-酯
公开(公告)号：US20090105470A1
公开(公告)日：2009-04-23
申请号：US11884678
申请日：2006-02-06
申请人： Rakesh Ratnam , Mohammed Mofizuddin , Sundeep Aurora
发明人： Rakesh Ratnam , Mohammed Mofizuddin , Sundeep Aurora
IPC分类号： C07H23/00
CPC分类号： C07H1/00 , C07H13/00
摘要： A method is disclosed for regioselective synthesis of sucrose-6-acetate via formation of a novel sucrose-tin adduct using sucrose and DBTO. The novel tin adduct can be represented by a formula (6-O-sucrose)-O—Snbutyl.sub.2-O-(6-O-sucrose) or as 1,3.(di O-sucrose) dibutyl stannylene. The adduct is acylated to yield sucrose-6-acetate or sucrose-6-benzoate as major product.
摘要翻译：公开了通过使用蔗糖和DBTO形成新的蔗糖 - 锡加合物来区域选择性合成蔗糖-6-乙酸酯的方法。新的锡加合物可以由式（6-O-蔗糖）-O- Snbutyl2-O-（6-O-蔗糖）或1,3（二O-蔗糖）二丁基亚锡来表示。将加合物酰化生成蔗糖-6-乙酸酯或蔗糖-6-苯甲酸酯作为主要产物。

14. 发明申请

US20090030193A1 Synthesis of Vilsmeier Haack Reagent from Di(Trichlo-Romethyl) Carbonate for Chlorination Reaction 审中-公开
标题翻译：用于氯化反应的二（三氯甲基）甲酸酯的Vilsmeier Haack试剂的合成
公开(公告)号：US20090030193A1
公开(公告)日：2009-01-29
申请号：US11919827
申请日：2006-04-28
申请人： Rakesh Ratnam , Sundeep Aurora , Shrikant Kulkarni
发明人： Rakesh Ratnam , Sundeep Aurora , Shrikant Kulkarni
IPC分类号： C13K13/00
CPC分类号： C07H5/02 , C07B39/00 , C07C249/02 , C07C251/30
摘要： A process of preparation of Vilsmeier-Haack reagent is provided where di(trichloromethyl) carbonate reacts with N,N-dimethylformamide to form a Vilsmeier reagent, which can be used efficiently for chlorination of sucrose-6-acetate or sucrose-6-benzoate and other sucrose acylates. This process has application in the process for preparation of 1-6-Dichloro-1-6-DIDEOXY-β-Fructofuranasyl-4-chloro-4-deoxy-galactopyranoside.
摘要翻译：提供Vilsmeier-Haack试剂的制备方法，其中碳酸二（三氯甲基）酯与N，N-二甲基甲酰胺反应形成维尔斯迈尔试剂，可有效地用于氯化蔗糖-6-乙酸酯或蔗糖-6-苯甲酸酯，其他蔗糖酰化物。该方法可用于制备1-6-二氯-1,6-二脱氧-β-呋喃果基-4-氯-4-脱氧 - 吡喃半乳糖苷的方法。

15. 发明申请

US20080300391A1 Acid Mediated Deacylation of 6-0-Trichlorogalactosurcrose to Trich-Lorogalactosucrose 审中-公开
标题翻译： 6-0-三氯半乳糖的酸介导的脱酰基作用到三萜半乳糖
公开(公告)号：US20080300391A1
公开(公告)日：2008-12-04
申请号：US12083859
申请日：2006-10-17
申请人： Rakesh Ratnam , Sundeep Aurora , Batchu Chandrashekar , Anandangowda Patil
发明人： Rakesh Ratnam , Sundeep Aurora , Batchu Chandrashekar , Anandangowda Patil
IPC分类号： C07H1/00
CPC分类号： C07H1/00 , C07H1/06 , C07H5/02 , C07H13/04
摘要： A process is described for acid mediated deacylation of acyl derivatives of chlorinated sucrose compounds comprising generating a predominantly organic phase condition in a process stream requiring deacylation treatment but allowing an optimum quantity of water content which is capable of participating in a hydrolysis reaction; this objective being achieved for the said process stream by following steps of (a) adding to it alcoholic solvent in an amount such that water content of final reaction mixture is between about 5% to 0.5%, (b) adding acid chloride to the same (c) adjusting the pH to 4 by adding acetate buffer in a methanolic solution and, (d) stirring the reaction until deacylation is complete. This process can be integrated in a process for production of a chlorinated compound, involving use of dimethylformamide during the process, to achieve deacylation without decomposition of dimethylformamide as well as the chlorinated sucrose product.
摘要翻译：描述了用于酸介导的氯化蔗糖化合物的酰基衍生物的脱酰基的方法，其包括在需要脱酰基处理的工艺流中产生主要有机相条件，但允许最佳量的能够参与水解反应的水含量; 通过以下步骤（a）向醇溶剂中加入一定量使得最终反应混合物的水含量在约5％至0.5％之间的量，（b）向其中加入酰氯，（c）通过在甲醇溶液中加入乙酸盐缓冲液将pH调节至4，和（d）搅拌反应直到完全脱酰基化。该方法可以整合到生产氯化化合物的方法中，涉及在该方法中使用二甲基甲酰胺，以达到脱酰基化而不分解二甲基甲酰胺以及氯化蔗糖产物。

16. 发明授权

US07951937B2 Process for purification of trichlorogalactosucrose based on direct extraction in organic solvent from reaction mixture followed by evaporative removal of solvent 失效
标题翻译：基于在有机溶剂中从反应混合物中直接萃取，然后蒸发除去溶剂，纯化三氯半乳糖蔗糖的方法
公开(公告)号：US07951937B2
公开(公告)日：2011-05-31
申请号：US11991144
申请日：2006-08-29
申请人： Rakesh Ratnam , Sundeep Aurora , Batchu Chandrasekhar
发明人： Rakesh Ratnam , Sundeep Aurora , Batchu Chandrasekhar
IPC分类号： C07H1/06 , C07H1/08
CPC分类号： C07H3/04 , C07H5/02
摘要： A process of azeotropic removal of dimethylformamide, abbreviated as DMF, from a process stream containing DMF requiring its removal, is described wherein the said Process Stream being obtained in a process for preparation of 4,1′,6′ trichlorogalactosucrose, abbreviated as TGS, or TGS-6-ester including TGS-6-acetate or TGS-6-benzoate, comprising steps of (a) evaporation of the said process stream under reduced pressure to a concentrate to effect removal of a part of DMF azeotropically, (b) diluting the concentrate obtained at the end of step (a.) of this claim with water, preferably to about 5 to 10 times the volume of the said concentrate, and (c) repeating the cycles of evaporation under reduced pressure and dilution with water for more number of times until content of DMF in the concentrated mass is reduced to 0.5% or less of the concentrate.
摘要翻译：描述了从含有需要其去除的DMF的工艺流中共沸除去二甲基甲酰胺（缩写为DMF）的方法，其中所述方法流是在制备4,1'，6'-三氯半乳糖，缩写为TGS的方法中获得的，或TGS-6-酯，包括TGS-6-乙酸酯或TGS-6-苯甲酸酯，包括以下步骤：（a）将所述工艺流在减压下蒸发至浓缩物以共沸除去一部分DMF，（b）用水稀释在该权利要求书的步骤（a）结束时获得的浓缩物，优选至少为所述浓缩物体积的约5至10倍，和（c）在减压下重复蒸发循环并用水稀释将浓缩物质中的DMF的含量降低至浓缩物的0.5％以下的次数更多。

17. 发明申请

US20100228020A1 Novel Chlorination Reagent and a Novel Process for Chlorination of Sugars Using Thionyl Chloride 审中-公开
标题翻译：新型氯化试剂和使用亚硫酰氯氯化氯的新方法
公开(公告)号：US20100228020A1
公开(公告)日：2010-09-09
申请号：US12224324
申请日：2007-02-28
申请人： Rakesh Ratnam , Sundeep Aurora , Mohammed Mofizuddin
发明人： Rakesh Ratnam , Sundeep Aurora , Mohammed Mofizuddin
IPC分类号： C07H13/02 , C07H1/00
CPC分类号： C07H1/00 , C07H5/02 , C07H13/02 , C07H15/00
摘要： Preparation of chlorinating reagent or chlorination reaction itself for use in a reaction such as production of high intensity sweetener trichlorogalactosucrose (TGS) from partially protected sucrose, comprising reaction of dimethylformamide (DMF) with thionyl chloride or another sulphur containing inorganic acid chlorides including sulphuryl chloride is faced with a problem of prolific release of gaseous by-products, that at times may lead to violent explosion also. This problem is solved by innovative addition of solid powder inert to the constituents of the chlorination reaction mixture to the reaction, or by adding DMF to acid chloride solution in that order. The invention also leads to use of isolated solid Vilsmeier reagent being used for chlorination in a solvent other than DMF making it possible to avoid altogether problems arising from use of DMF which include irrecoverable loss in alkaline as well as acid conditions, interference in crystallization of TGS and the like.
摘要翻译：制备氯化试剂或氯化反应本身用于反应，例如从部分保护的蔗糖生产高强度甜味剂三氯半乳糖（TGS），包括二甲基甲酰胺（DMF）与亚硫酰氯或另一种含硫的无机酰氯（包括磺酰氯）的反应，面临气体副产品多产释放的问题，有时也可能导致剧烈的爆炸。通过将氯化反应混合物的成分惰性的固体粉末添加到反应中，或者通过向该酰氯溶液中依次加入DMF来解决这个问题。本发明还导致使用分离的固体维尔斯迈尔试剂用于在DMF以外的溶剂中进行氯化，使得可以避免使用DMF引起的一切问题，其包括在碱性和酸性条件下不可恢复的损失，TGS的结晶干扰等等。

18. 发明申请

US20100190975A1 Method for purification of chlorinated sucrose derivatives by solvent extraction 审中-公开
标题翻译：通过溶剂萃取法纯化氯化蔗糖衍生物的方法
公开(公告)号：US20100190975A1
公开(公告)日：2010-07-29
申请号：US11921183
申请日：2006-05-26
申请人： Rakesh Ratnam , S. P. Raviraj , Sundeep Aurora
发明人： Rakesh Ratnam , S. P. Raviraj , Sundeep Aurora
IPC分类号： C07H1/06
CPC分类号： C07H5/02 , C07H1/06
摘要： A process is described for extractive isolation and purification of Trichlorogalactosucrose from impurities from a composition substantially free from N-N Dimethylformamide (DMF) comprising a first extractive separation by adjusting aqueous to a mixture of organic solvents in the composition to a certain ratio of aqueous to organic phase, extracting the aqueous layer of this step by a single organic solvent, followed by saturation of the aqueous layer by salt and ultimately extracting TGS in the organic layer.
摘要翻译：描述了一种用于从基本上不含二甲基甲酰胺（DMF）的组合物的杂质中萃取分离和纯化三氯半乳糖蔗糖的方法，所述组合物包含通过将组合物中的水与有机溶剂的混合物调节至一定比例的水相与有机相的第一萃取分离通过单一有机溶剂提取该步骤的水层，然后用盐饱和水层，最终在有机层中萃取TGS。

19. 发明申请

US20100056773A1 DECOLORIZATION OF PROCESS STREAMS BY CHEMICAL OXIDATION IN THE MANUFACTURE OF TRICHLOROGALACTOSUCROSE 审中-公开
标题翻译：化学氧化在三氯蔗糖生产中的工艺流程分解
公开(公告)号：US20100056773A1
公开(公告)日：2010-03-04
申请号：US12448791
申请日：2008-01-02
申请人： Batchu Chandrasekhar , Andanagouda Sharanappagouda Patil , Rakesh Ratnam , Sundeep Aurora
发明人： Batchu Chandrasekhar , Andanagouda Sharanappagouda Patil , Rakesh Ratnam , Sundeep Aurora
IPC分类号： C07H1/00
CPC分类号： C07H17/04 , C07H5/02 , C13B20/08
摘要： A process is described in which decolorization of solutions or reaction mixtures containing trichlorogalactosucrose or 6-acetyl trichlorogalactosucrose is achieved described by bubbling ozone. The method can be used at various stages in the process of production and with or without a combination with other adsorbents for colour removal.
摘要翻译：描述了一种方法，其中通过鼓泡臭氧描述了含有三氯半乳糖蔗糖或6-乙酰基三氯乳糖蔗糖的溶液或反应混合物的脱色。该方法可以在生产过程中的不同阶段使用，并且可以与其它吸附剂组合使用以进行颜色去除。

20. 发明申请

US20090264640A1 Recovery of dimethylformamide and other solvents from process streams of manufacture of trichlorogalactosucrose 审中-公开
标题翻译：从三氯蔗糖生产工艺流中回收二甲基甲酰胺和其他溶剂
公开(公告)号：US20090264640A1
公开(公告)日：2009-10-22
申请号：US12227595
申请日：2007-05-16
申请人： Rakesh Ratnam , Sundeep Aurora , n/a Subramaniyan
发明人： Rakesh Ratnam , Sundeep Aurora , n/a Subramaniyan
IPC分类号： C07H3/04 , C07C231/24
CPC分类号： C07H1/06 , B01D15/3804 , B01J20/285 , C07C231/24 , C07C233/03
摘要： This invention comprises an improved process for recovery and purification of DMF from an aqueous process stream containing DMF with or without inorganic impurities, particularly from process stream of a process of manufacture of the high intensity sweetener Trichlorogalactosucrose, by adsorption on an adsorbent having selective affinity towards dimethylformamide, followed by elution in pure form by eluting by an appropriate eluent, including methanol.
摘要翻译：本发明包括从含有或不含无机杂质的DMF的水性工艺流中回收和纯化DMF的改进方法，特别是通过在具有选择性亲和力的吸附剂上吸附制备高强度甜味剂三氯半乳糖蔗糖的工艺流二甲基甲酰胺，然后通过包括甲醇在内的合适的洗脱液进行洗脱纯化。

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