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Method for purification of chlorinated sucrose derivatives from reaction mixture by chromatography

A technology of chlorinated sucrose and chromatographic chromatography, which is applied to the preparation of sugar derivatives, sugar derivatives, sugar derivatives, etc., can solve problems such as expensive, cumbersome technology, and inconvenient

Inactive Publication Date: 2011-04-13
V B MEDICARE PVT LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, these techniques are cumbersome, inconvenient and expensive for practical application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach

[0037] a) The neutralized reaction mass can be concentrated until the water is completely removed and the obtained mixture of DMF, inorganic salts and chlorinated sucrose derivatives is used for column chromatography using hydrophobic silica.

[0038] b) The neutralized reaction material can be extracted into a water-insoluble or slightly water-soluble solvent such as ethyl acetate, methyl ethyl ketone, butyl acetate, etc., and then concentrated to remove the organic solvent. The resultant liquid slurry with DMF and chlorinated sucrose derivatives was purified using column chromatography on hydrophobic silica.

[0039] c) The neutralized material can be concentrated until the water is completely removed, then extracted into an organic solvent such as ethyl acetate, butyl acetate, methyl ethyl ketone, etc., then concentrated to remove the organic solvent and column chromatography using hydrophobic silica The obtained slurry was purified.

[0040] On an industrial scale, the co...

Embodiment 1

[0045] The preparation of embodiment 1, TGS-6-acetate

[0046] At a temperature of 20°C, 252.8g of PCl was mixed with stirring 5 Add slowly to 700 L of DMF in a glass lined reactor. The Vilsmeier reagent thus formed was then cooled to 0°C. 80 kg of 75% pure sucrose-6-acetate dissolved in DMF was slowly added with stirring. During the addition process, the temperature was kept at 0-5°C. Modifications in place of sucrose-6-acetate may include any other acylation product or any other ester; and thus appropriate subsequent modifications / changes may be made.

[0047] After addition of sucrose-6-acetate, the temperature was allowed to rise to room temperature, usually about 30-35°C, and stirred for 60 minutes. The reaction mass was then heated to 85°C for 60 minutes and further heated to 100°C for 6 hours. The reactant was heated again to 115° C. and maintained for 90 minutes, and then the reactant was neutralized to pH 6.5˜7.0 with 7% ammonia water. The total volume of the neut...

Embodiment 2

[0048] Embodiment 2, the direct purification of neutralized material after the chlorination reaction

[0049] The neutralized material containing TGS-6-acetate from Example 1 was filtered on a filter press to remove all suspended matter and obtain a clear filtrate. The reaction mixture was a liquid composition with 20% DMF. 200 kg of silanized silica gel (hydrophobic) was slurried in phosphate buffer, pH 9.5-10.5, and loaded into an SS column (two alternative methods for silanized silica need to be described here). The silica gel was left in the buffer for 12 hours without drying out. Column equilibration was initiated by passing approximately 600 L of pH 10.5-11.0 buffer. 250 L of filtered neutralized material was loaded on top of the silica gel bed packed into the SS column. Apply 0.5~0.8kg / cm 2 Slight air pressure to push the neutralized material through the silica gel bed. The flow rate from the column was adjusted to 200 LPH. When the neutralization material passed ...

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PUM

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Abstract

A chromatographic process of DMF removal from an aqueous composition is described comprising its loading on a column of hydrophobic fixed bed adsorbent and eluting out DMF with an aqueous alkaline buffer. This method is useful to remove DMF as a process of general application wherever simultaneous removal and isolation of DMF is desired from an organic molecule which is not an organic solvent, is soluble in DMF. This method can be used for simultaneous removal of DMF from reaction mixtures and isolation of Trichlorogalactose (TGS) or TGS-6-acetate in a process of production of TGS.

Description

technical field [0001] The present invention relates to a method for separating and purifying 1'-6'-dichloro-1'-6'-dideoxy-β-fructofuranose-4-chloro-4-deoxy-galactopyranoside from a reaction mixture (TGS) and other chlorinated sucrose derivatives methods and new strategies. Background technique [0002] The preparation of chlorinated sucrose is a complex process due to the need to perform chlorination at less selective reactive sites on the sucrose molecule in competition with highly selective reactive sites. This objective is usually achieved by a process that involves essentially protecting the hydroxyl group in the pyranose ring of the sugar molecule by using various protecting reagents such as alkyl / aryl anhydrides, acid chlorides, orthoesters, etc. , then chlorinated the protected sucrose at the desired position (1'-6' and 4) to give the acetyl derivative of the product, which was then deacetylated to give the desired product 1'-6-dichloro-1 -6-dideoxy-β-fructofuranos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/06C07H5/02C07H13/06B01D15/08
CPCC07H1/06B01J20/285B01J20/287B01J20/3217B01J20/283C07H5/02B01J20/261B01J20/265C07H1/00C07K1/16C07K1/14
Inventor 萨布拉曼亚姆切塔纳拉南·拉克什奥萝拉·森迪普
Owner V B MEDICARE PVT LTD
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