cas 56038-13-2, Sucralose | Articles data

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Bioconversion of sucralose-6-acetate to sucralose using immobilized microbial cells
Bioconversion of sucralose-6-acetate to sucralose, an artificial sweetener has been carried out using Arthrobacter sp. (ABL) and Bacillus subtilis (RRL-1789) strains isolated at IIIM, Jammu, India. Biotransformation of sucralose-6-acetate to sucralose involves use of microbial whole cells, immobilized whole cells and immobilized whole cell bioreactor. Immobilized whole cells packed bed reactor has shown much superior biotransformation process in aqueous system using green technology, where purification of the final product is not required. The final sucralose bioproduct was directly concentrated under vacuum to get white crystalline powder. The immobilized whole cell bioreactor was used for more than three cycles continuously, thus provided much cheaper, less time consuming and easy down streaming process. Moreover, the method does not require any purification steps, which is otherwise requisite for presently available methods for sucralose production, resulting in even lower cost of overall process.
Chaubey, Asha,Raina, Chand,Parshad, Rajinder,Rouf, Abdul,Gupta, Pankaj,Taneja, Subhash C.
p. 81 - 86
(2013)
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A chlorinating agent preparation method and its method of preparing sucralose
The invention provides a preparation method of a novel chlorinating agent, which includes following steps: 1) dissolving an N,N-disubstituted formamide derivative in a nonprotic organic solvent and cooling the solution to 0 DEG C with stirring; 2) adding dropwisely thionyl chloride or oxalyl chloride to the solution obtained in the step 1) with dropwise addition temperature controlled to be 10-20 DEG C, heating the solution to 20-40 DEG C when the dropwise addition is finished, and performing a reaction for 1-2 h and cooling the solution to room temperature after the reaction finished; and 3) filtering the reaction product to obtain the chlorinating agent. The preparation method increases selectivity of a chlorination reaction, wherein the chlorination is carried out in a stepwise temperature increasing manner, so that yield of chlorination is greatly increased. The method solves difficulty of separation of the sucralose and reduces the production cost of the sucralose.
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Page/Page column 5-6

(2018/09/02)

Recrystallization method of sucrose-6-acetate and applications thereof
The invention discloses a recrystallization method of sucrose-6-acetate, and applications thereof. The recrystallization method comprise following steps: a solvent is added into a sucrose-6-acetate mixture obtained via sucrose esterification; and stirring, dissolving, filtering, and drying are carried out so as to obtain sucrose-6-acetate, wherein the solvent is a mixture of a nitrile solvent and an ether solvent. The recrystallization method is capable of increasing sucrose-6-acetate purity, and reducing adverse influences on subsequent chlorination.
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Paragraph 0052; 0053; 0058

(2017/09/01)

A method of preparing sucralose
The invention provides a modified synthetic technology for sucralose. Trimethyl orthoacetate and excess sucrose are subjected to a cyclization reaction in DMF for improving the utilization rate of high-price trimethyl orthoacetate, then a low-polarity solvent is added into the reaction solution so as to enable unreacted sucrose to be crystallized and precipitated from the reaction solution, after separation, the purity of sucrose-4,6-cyclic ester in the reaction solution is 95% or more; then through ring opening and acyl migration, the content of sucrose-6-ester in the reaction solution is 90% or more; the DMF solution of sucrose-6-ester is subjected to dewatering processing and then directly subjected to a next-step chlorination reaction, and the chlorination product is subjected to deacetylation by sodium methoxide so as to obtain sucralose; and unreacted sucrose can be recovered for using, and the reaction total yield, calculated based on sucrose, can reach 37% or more. Compared with conventional technology, the utilization rate of trimethyl orthoacetate in the technology is improved by 10% or more.
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Paragraph 0074; 0075

(2016/10/07)

Deacylating method of sucralose-6-acetate
The invention discloses a deacylating method of sucralose-6-acetate, comprising the following steps: adding sucralose-6-acetate into methanol solution of sodium methylate, reacting at 58-62 DEG C for 3-5 hours, vacuum distilling and recycling methanol, and washing obtained solid with ethyl acetate to obtain sucralose. Compared with existing deacylating methods of sucralose-6-acetate, the method of the invention can be used to provide significant deacylating effect, and the yield of sucralose after deacylating is up to higher than 85%.
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Paragraph 0013; 0014

(2016/12/01)

Trichlorosaccharose-6-acetate continuous deacetyl systems trichlorosaccharose method
The invention provides a method for preparing sucralose by continuously deacetylating sucralose-6-acetate. According to the method, in the presence of a basic catalyst, the sucralose-6-acetate is deacetylated to generate the sucralose, the catalyst is added in a segmented mode according to pH of a reaction solution, a novel reactor is adopted so that the catalyst can be rapidly mixed and dispersed, and the reaction temperature is easy to control. The synthetic sucralose has the advantages that residual quantity of the sucralose-6-acetate is small, the content of dichloro sucrose is low, the usage amount of the catalyst is small, the yield of the sucralose is high, continuous operation is achieved, the production cycle is shortened, and production cost is saved.
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Paragraph 0023; 0024; 0025; 0026

(2017/03/17)

CHLORINATION OF SUCROSE-6-ESTERS
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.
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Page/Page column 19-24

(2015/07/07)

PROCESS FOR THE PREPARATION OF SUCRALOSE
The present invention provides a method for preparing colorless sucralose, wherein 4,1′,6′-trichloro-4,1′,6′-trideoxy-galacto sucrose-6- acetate containing colored impurities formed during chlorination of sucrose-6-acetate is treated with sodium hypochlorite, where sodium hypochlorite acts both as a decolorizing agent and as a reagent for the ester hydrolysis.
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Paragraph 0016

(2013/03/26)

Method of sucralose synthesis yield
The invention discloses a method for improving the yield of sucralose, including reacting sucrose to produce sucrose-6-acetate in the existence of an azo reagent as a catalyst and acetic acid as an acylating agent in a proper solvent; then reacting sucrose-6-acetate with a proper chlorinating agent to produce sucralose-6-acetate in a non-proton polar solvent with TCA as a catalyst; and at last, alcoholyzing sucralose-6-acetate in KOH/methanol to obtain sucralose.
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Page/Page column 6

(2011/02/26)

Oral Solid Dosage Form Containing Nanoparticles and Process of Formulating the Same Using Fish Gelatin
An oral solid dosage form containing nanoparticles is made by (a) reducing the particle size of at least one pharmaceutically active ingredient dispersed in a solution containing fish gelatin to form a nanosuspension and (b) freeze-drying the nanosuspension of step (a) to form the oral solid dosage form.
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(2011/04/18)

Novel Preparation of 6-O-Acyl Chlorosucrose from Anhydrous Cholorinated Reaction Mass
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.
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Page/Page column 2-3

(2010/07/04)

Novel Chlorination Reagent and a Novel Process for Chlorination of Sugars Using Thionyl Chloride
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.
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Page/Page column 5-6

(2010/09/17)

PROCESS FOR REMOVING DIMETHYLAMINE
A process for removing dimethylamine (DMA) before and/or during and/or after deacylation in a reaction vessel of a feed stream comprising a sucralose-6-acylate resulting from the chlorination of a sucrose-6-acylate in the presence of dimethyl formamide (DMF), wherein the deacylation is conducted at a first set of conditions of temperature, pH and pressure, the process comprising: (a) providing a side stream loop from and to the reaction vessel; (b) adjusting the conditions of one or more of temperature, pH, and pressure in the loop, and setting the flow rate through the loop, to remove DMA while minimising carbohydrate degradation.
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Page/Page column 14-15

(2010/11/03)

PURIFICATION OF TERTIARY FORMAMIDE CONTAMINATED WITH TERTIARY ACETAMIDE
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).
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Page/Page column 14

(2011/01/12)

Removal of pyridine and pyridine analogs from reaction mass containing sucrose esters
A process of removal of pyridine or a pyridine analogue from a composition or a Process Stream in a process of production of 4,1′, 6′ trichlorogalactosucrose is described comprising reacting pyridine with an acid, the said acid being used preferably in gaseous form, achieving complete precipitation of the salt of pyridine in higher alcoholic solvents and non-polar solvents, filtering off the precipitate of the said salt of pyridine to achieve removal of pyridine from the reaction system and optionally regenerating and recovering pyridine by reacting the said salt with alkali.
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Page/Page column 3

(2010/09/07)

DECOLORIZATION OF PROCESS STREAMS BY CHEMICAL OXIDATION IN THE MANUFACTURE OF TRICHLOROGALACTOSUCROSE
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.
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Page/Page column 2

(2010/04/23)

Process to Prepare Sucralose
The present invention relates to a process to prepare sucralose. More particularly the said process relates to the production of sucralose, chemically known as, 6-Dichloro-1,6-dideoxy-β-D-fructofuranosyl-4-chloro-4-deoxy-alpha-D-galactopyranoside of formula (1)
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Page/Page column 4

(2010/08/07)

Process for purification of sucralose
The present invention relates to a process for the purification of Sucralose of formula (I) which comprises acetylation of substantially impure Sucralose to its penultimate intermediate 4,1′,6′-trichloro-4,1′,6′-trideoxy galactosucrose penta-acetate (TOPSA) of formula (VI) followed by purification of TOPSA and then deacetylation of purified TOPSA.
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Page/Page column 6

(2010/07/02)

PROCESS FOR SYNTHESIZING AND PURIFYING SUCRALOSE
The present invention discloses a process for synthesizing sucralose, which comprises reacting sucrose with acetic anhydride in the solvent of a N-amide compound in the presence of an organic complex alkali metal salt catalyst to produce sucrose-6-acetate, and then chlorinating and deacetylating the sucrose-6-acetate to give sucralose. The present invention also discloses a process for purifying sucralose, which comprises purifying crude sucralose with one or more organic solvents to obtain purified sucralose.
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(2010/10/05)

Process for the Preparation of Sucralose
A process for the preparation of a sucralose which comprises the steps of: reacting a sucrose with a chlorinating reagent in a non-proton type polar solvent to form chlorinated sucrose (4,6,1′,6′-tertchloro-4,6,1′,6′-tertdeoxylgalactosucrose); reacting the chlorinated sucrose and a carboxylate salt to form sucralose-6-acetate in a dissolvent; and finally de-acylating the sucralose-6-acetate in sodium methoxide/methanol system and then the desired product sucralose is thereby produced. The present invention is generally related to the industrial production of sucralose with the advantages of mild reaction conditions, high yield rate, and brief operation.
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Page/Page column 3

(2009/09/26)

METHOD FOR THE PRODUCTION OF SUCRALOSE
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).
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Page/Page column 8

(2009/10/06)

METHOD FOR THE PRODUCTION OF SUCRALOSE
The present invention provides a method for producing sucralose from a feed stream resulting from the chlorination of a sucrose-6-acylate in a reaction vehicle. The feed stream includes a sucralose-6-acylate, the reaction vehicle, water, and salts. The salts include one or more selected from the group consisting of alkali metal chlorides, alkaline earth metal chlorides and ammonium chloride. The method includes: (i) deacylation of the sucralose-6-acylate by treatment with a base to afford a product stream comprising sucralose;(ii) partial removal of water and, optionally, reaction vehicle from the product stream of (i) in order to cause precipitation of the salts from the product stream;(iii) removal of the precipitated salts from the product stream of (ii); and(iv) isolation of sucralose from the product stream of (iii).
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Page/Page column 5-6

(2009/10/30)

PROCESS FOR PURIFICATION OF TRICHLOROGALACTOSUCROSE BASED ON DIRECT EXTRACTION IN ORGANIC SOLVENT FROM REACTION MIXTURE FOLLOWED BY EVAPORATIVE REMOVAL OF SOLVENT
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.
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Page/Page column 2

(2009/05/28)

Process for Preparing Sucrose-6-ester
This invention relates to a method for preparing a sucrose-6-ester. The method includes (i) reacting sucrose with a N,N-dimethylcarboxamide dimethyl acetal in an inert aprotic solvent to form a cyclic acetal of formula (I): wherein R is C1-C6 alkyl, C3-C20 cycloalkyl, C1-C20 heterocycloalkyl, aryl, or heteroaryl; and (ii) subjecting the cyclic acetal to a mild acidic or neutral hydrolysis to provide a sucrose-6-ester of formula (II):
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Page/Page column 3

(2008/06/13)

PROCESS FOR THE PREPARATION OF SUCRALOSE BY THE CHLORINATION OF SUGAR WITH TRIPHOSGENE (BTC)
In one embodiment of the invention a method to prepare sucralose-6-acylate through chlorinating sucrose-6-acylater by BTC in the process of sucralose preparation is disclosed. In this embodiment a Vilsmeier reagent is firstly prepared below 0° C. by dissolving BTC in DMF or in component solvent, containing DMF, toluene, dichloroethane, chloroform and carbon tetrachloride. Consequently, sucrose-6-ester was chlorinated by Vilsmeier reagent. BTC can also be dissolved in one or several organic solvent such as toluene, dichloroethane, chloroform and carbon tetrachloride, and added to a DMF solution of sucrose-6-acylate for chlorination. Sucralose was prepared through de-esterifying the obtained sucralosed 6-ester using sodium methoxide/methanol or sodium ethoxide/ethanol.
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Page/Page column 2

(2008/06/13)

PROCESS FOR THE PREPARATION OF SUCRALOSE BY THE DEACYLATION OF TRICHLOROSUCROSE-6-ETHYL ESTER
The present invention discloses a process for the preparation of sucralose by the deacylation of trichlorosucrose-6-ethyl ester, wherein the deacylation reaction is performed in an alcohol solvent in the presence of organic base catalyst, so as to obtain sucralose.
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Page/Page column 1-2

(2008/12/08)

Salts Assisted Selective Extraction Of 6-Acetyl- 4,1' , 6' Trichlorogalactosucrose And 4,1', 6' Trichlorogalactosucrosse From Aqueous Reaction Mixture
A process is described to increase efficiency of extraction of 4,1′,6′ trichlorogalactosucrose (TGS) from aqueous solution by addition of salt. The invention helps in reducing the quantity of solvent needed for achieving substantial extraction. The invention also leads to extraction of TGS substantially free from polar impurities.
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Page/Page column 2

(2008/12/05)

METHOD FOR CRYSTALLIZING SUCRALOSE
The present application discloses a method for crystallizing sucralose, which comprises using a mixed solvent, which comprises two solvents with different boiling points, wherein the solvent with lower boiling point has higher solubility to sucralose than the solvent with higher boiling point. The method of the present invention has the advantages of low cost, high yield, mild processing conditions, stable quality, simple apparatuses and so on.
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Page/Page column 2

(2008/12/06)

IMPROVED SUCRALOSE PRODUCTION METHOD
There is provided a method for the production of sucralose from a feed stream resulting from the chlorination of a sucrose-6-acylate in a reaction vehicle, said feed stream comprising a sucralose-6-acylate, the reaction vehicle, and by-products including high molecular weight coloured material, said method comprising: deacylation of the sucralose-6-acylate by treatment with a base to afford sucralose, and, before or after said deacylation, removal of the reaction vehicle and isolation of the sucralose characterised in that immediately before the removal of the reaction vehicle, the reaction stream is subjected to a precipitation step comprising treatment with a metal or ammonium hydroxide and carbon dioxide to form a precipitate of the corresponding metal or ammonium carbonate in which at least a portion of said high molecular weight coloured material is trapped, followed by separation of said precipitate.
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Page/Page column 8-9; 10-11; 12-13

(2008/12/07)

METHOD FOR CRYSTALLIZING SUCRALOSE
The present application discloses a method for crystallizing sucralose, which uses an alcohol solvent or a mixed solvent of alcohol and other solvent(s) in the crystallization of sucralose.
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Page/Page column 1-2

(2008/12/08)

METHOD OF PRODUCING SUCRALOSE
A method of producing sucralose is disclosed. The method of producing sucralose comprises the steps of preparing a compound (6, 1', 6'-tri- 0 -tritylsucrosepenta- acetate) by reacting sucrose, which is a starting material, with a tritylating agent to form a reaction product, and then reacting the reaction product with acetic anhydride (step 1); preparing a compound (2, 3, 4, 3', 4'-penta- 0 -acetylsucrose) by reacting the compound prepared in step 1 with hydrogen chloride gas having the same equivalent amount as the compound (step 2); preparing a compound (2, 3, 6, 3', 4'-penta- 0 -acetylsucrose) by isomerizing the compound prepared in step 2, under a base catalyst (step 3); preparing a compound (4, 1', 6'-trichloro- 4, 1', 6'-trideoxy-2, 3, 6, 3', 4'-penta- 0 -acetyl-galactosucrose) by chlorinating the compound prepared in step 3 (step 4); and preparing 4,1, 6'-trichloro-4, 1', 6'-trideoxygalactosucrose by deacetylating the compound prepared in step 4, and then filtering the deacetylated compound using a cation exchange resin (step 5).
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Page/Page column 11-12

(2008/12/08)

PROCESS FOR THE PREPARATION OF SUCROSE-6-ESTER BY ESTERIFICATION IN THE PRESENCE OF SOLID SUPERACID CATALYST
One embodiment of the present invention is a process of making sucrose-6-ester from sucrose by transesterification in the presence of a solid super acid catalyst such as SO42?—TiO2/Al2O3 or SO42?—TiO2. The sucrose-6-acetate is then chlorinated to afford sucralose-6-acetate, using BTC or thionyl chloride. Sucralose-6-acetate is converted into TPSGA for the purpose of purification. TPSGA is de-esterified by sodium methoxide/methanol or sodium ethoxide/ethanol to give sucralose.
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Page/Page column 2-3

(2008/06/13)

AN IMPROVED PROCESS FOR THE PREPARATION OF SUCRALOSE OF HIGH PURITY
The present invention relates to an improved process for the preparation of Sucralose having purity of at least 99.6% comprising steps of (i) dissolving substantially impure Sucralose in water; (ii) treating the solution obtained in step (i) with a partially water immiscible solvent; (iii) washing the said solvent phase obtained in step (ii) with an amount of water sufficient to remove polar impurities; (iv) crystallizing the product from partially water immiscible solvent; (v) recrystallizing the solid obtained in step (iv) from water.
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Page/Page column 7-8

(2008/06/13)

Novel chlorination process for preparing sucralose
A process for preparing a sucralose-6-ester, a key intermediate to sucralose. The process contains (a) creating a heterogeneous mixture comprising a first phase comprising a sucrose-6-ester and a second phase comprising a chlorinating reagent; and (b) reacting the sucrose-6-ester with the chlorinating reagent, to prepare a sucralose-6-ester. In addition, processes for preparing sucralose from sucrose-6-esters are provided.
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Page/Page column 9

(2009/01/20)

ACID MEDIATED DEACYLATION OF 6-0-TRICHLOROGALACTOSUCROSE TO TRICH-LOROGALACTOSUCROSE.
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.
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Page/Page column 8-11

(2008/06/13)

Process for Purification of 6 Acetyl 4,1', 6' Trichlorogalactosucrose and 4,1', 6' Trichlorogalactosucrose by Chromatography on Silanized Silica Gel
A reverse phase column chromatographic process of purification of 6-acetyl-4,1′,6′trichlorogalactose and 4,1′,6′trichlorogalactose is described which uses silanized silica as stationary phase and water or predominatly aqeous mixture derived from water and small proportion of organic solvents as a mobile phase.
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Page/Page column 3-4

(2008/06/13)

PROCESS FOR THE PREPARATION OF A GLUCOSE DERIVATIVE
The present invention relates to an improved, safe, commercially viable, cost effective and eco friendly process for the preparation of 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose (Sucralose). The invention is directed towards the convenient synthesis of 2,3,4,3',4'-penta-O-acetyl sucrose (4-PAS) from 6,1',6'-tri-O-trityl-penta-O-acetyl sucrose ("TRISPA").
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Page/Page column 32

(2010/11/28)

Conversion of sucralose-6-ester to sucralose
The present disclosure provides a process for producing sucralose from a feed mixture of (a) sucralose-6-ester, such as 6-O-acyl-4,1′,6′-trichloro-4,1′,6′-trideoxygalactosucrose, (b) salt including alkali metal or alkaline earth metal chloride, (c) water, and (d) other chlorinated sucrose by-products, in a reaction medium comprising a tertiary amide, wherein said process comprises deacylating, either before or after removal of the tertiary amide, the sucralose-6-ester under active cooling to produce an aqueous solution comprising sucralose, salt including alkali metal or alkaline earth metal chloride, and other chlorinated sucrose by-products. Additionally, the sucralose may be recovered from the aqueous solution, such as by extraction followed by crystallization or by extractive techniques alone.
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Page/Page column 7; sheet 1; sheet 2; sheet 3; sheet 4; sheet 5

(2008/06/13)

MOLECULAR SEPARATION PROCESS IN VARIOUS STEPS OF PROCESS FOR PRODUCTION OF CHLORINATED SUGARS, THEIR PRECURSORS AND DERIVATIVES
This invention comprises novel application of a molecular separation process, including one or more of a membrane separation/filtration process comprising reverse osmosis, micro filtration, nanofiltration ultrafiltration and perevaporation and the like to several process streams obtained in process of production of for synthesis, purification or isolation of 1-6-Dichloro-1-6-DIDEOXY-β-Fructofuranosyl-4-chloro-4-deoxy-galactopyranoside (TGS), its precursors or its derivatives for achieving a separation of molecules in combination with conventional unit processes of separation.
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Page/Page column 10-12

(2008/06/13)

CHROMATOGRAPHIC PURIFICATION OF CHLORINATED SUCROSE
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Page 5

(2008/06/13)

METHODS FOR BUFFER STABILIZED AQUEOUS DEACYLATION
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.
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Page/Page column 16

(2008/06/13)

Production of sucralose without intermediate isolation of crystalline sucralose-6-ester
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.
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(2008/06/13)

Chlorination of sugars
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.
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(2008/06/13)

Selective acrylation of sugars
Sucrose or derivatives thereof such as esters are acylated at the 4'- and/or the 6-position by reaction with a donor acyl ester, e.g. a reactive ester of an alkanoic acid or benzoic acid, in the presence of lipase. Sucrose 6,4'-diesters so produced can be chlorinated and deacylated to produce the sweetener sucralose.
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(2008/06/13)

Sucrose derivatives
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(2008/06/13)

Process for the chlorination of sugars
Sugars and partly protected sugar derivatives are chlorinated by reaction of unprotected hydroxyl groups with thionyl chloride to form a persulphite followed by decomposition of the sulphite groups to form chlorosulphites, displacement of the chlorosulphite groups and insertion of chlorine atoms at one or more positions, characterised in that formation and displacement of the chlorosulphite groups and insertion of chlorine atoms is effected by reaction with thionyl chloride in an inert solvent in the presence of a quaternary salt of the general formula: wherein R1, R2 and R3, which may be the same or different, each represent a lower alkyl group, and R4 represents a hydrocarbon group with at least seven carbon atoms; and, when the sugar or partly protected sugar derivative has more than three unprotected hydroxyl groups, the process comprises the following stages: (a) reaction of the sugar or partly protected sugar derivative with thionyl chloride in the presence of pyridine to form a persulphite; (b) isolation of the polysulphite to remove free pyridine; and (c) reaction of the isolated polysulphite with thionyl chloride in an inert solvent or suspension medium in the presence of a quaternary salt of the general formula (I).
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(2008/06/13)

Selected removal of trityl groups from trispa
2,3,4,3',4'-penta-O-acetyl sucrose (4-PAS), a key intermediate in the preparation of sucralose, is prepared by the selective removal of trityl groups from 6,1', 6'-tri-O-trityl-penta-O-acetyl sucrose (TRISPA) in which a catalytic amount of an aralkyl chloride or hydrogen chloride is added to a solution of TRISPA is an inert organic solvent is hydrogenated in the presence of a hydrogenolysis catalyst such a platinum or palladium.
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(2008/06/13)