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Rectification and crystallization method of glucurolactone

A technology of glucuronolactone and seed crystals, which is applied in the field of medicine, can solve problems such as low product content, poor product crystal form, and difference in effect, and achieve the effect of ensuring crystal quality

Active Publication Date: 2011-10-19
JIANGSU TASLY DIYI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has obvious disadvantages. The product sticks to the wall during crystallization, and the product crystal form is poor. It is a white crystalline powder. The product content is not high, generally below 99%. Because the powder brings a lot of inconvenience to use and packaging, it is even different There are also differences in the effect of other crystal forms

Method used

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  • Rectification and crystallization method of glucurolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1, refining method of the present invention

[0038] Mix 500kg of cornstarch and 550kg of 75% nitric acid in a reaction kettle, add 10kg of sodium nitrite at the same time, and then react at 45°C for 5 hours. Kettle, carry out pressure hydrolysis at 0.25~0.28Mpa, about 135°C for 1 hour, after hydrolysis is complete, the hydrolyzate is concentrated in vacuum below 55°C to a concentration of about 45Be, and the concentrate is mixed with glacial acetic acid 250kg at 45°C for esterification, and kept for 16hrs , and then concentrate the esterification solution, the concentrated esterification solution was cooled and crystallized for 3 days, and centrifuged to obtain 105 kg of crude glucuronolactone.

[0039] Add 80kg of purified water into the decolorization kettle, and add 100kg of crude glucuronolactone under stirring condition. Raise the temperature to 85°C, add 5kg of activated carbon, decolorize for 15 minutes, heat filter, transfer the filtrate to a crysta...

Embodiment 2

[0040] Embodiment 2, refining method of the present invention

[0041] Mix 500kg of cornstarch and 550kg of 78% nitric acid in a reaction kettle, add 10kg of sodium nitrite at the same time, and then react at 45°C for 5 hours. Kettle, carry out pressure hydrolysis at 0.25~0.28Mpa, 135°C for 1 hour, after hydrolysis is complete, the hydrolyzate is concentrated in vacuum at a temperature lower than 55°C to a concentration of about 45Be, and the concentrate is mixed with 250kg of glacial acetic acid at 45°C for esterification, and kept for 15hrs. Then the esterified solution was concentrated again, and the concentrated esterified solution was cooled and crystallized for 3 days, and centrifuged to obtain 108 kg of crude glucuronolactone.

[0042] Add 100kg of purified water into the decolorization kettle, and add 100kg of powdered crude glucuronolactone under stirring conditions. Raise the temperature to 75°C, add 1kg of activated carbon, decolorize for 5 minutes, heat filter, tr...

Embodiment 3

[0043] Embodiment 3, refining method of the present invention

[0044] Mix 500kg of cornstarch and 550kg of 78% nitric acid in a reaction kettle, add 10kg of sodium nitrite at the same time, and then react at 45°C for 5 hours. Kettle, carry out pressure hydrolysis at 0.25~0.28Mpa, 138°C for 1 hour, after hydrolysis is complete, the hydrolyzate is concentrated in vacuum at a temperature lower than 55°C to a concentration of about 45Be, and the concentrate is mixed with 250kg of glacial acetic acid at 45°C for esterification, and kept for 16hrs. Then the esterified solution was concentrated again, and the concentrated esterified solution cooled and crystallized for 3 days, and centrifuged to obtain 106 kg of crude glucuronolactone.

[0045] Add 80kg of purified water into the decolorization kettle, and add 100kg of crude glucuronolactone under stirring condition. Raise the temperature to 80°C, add 3kg of activated carbon, decolorize for 10 minutes, heat filter, transfer the filtr...

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Abstract

The invention belongs to the field of pharmacy and relates to a rectification and crystallization method of glucurolactone. The rectification method comprises the following steps: (1) adding crude glucurolactone into a solvent for dissolution; (2) decoloring by adding activated carbon; (3) filtering, dropwise adding ethanol into a filtrate, and simultaneously cooling the filtrate; (4) adding crystal seeds in the cooling process, and stirring; and (5) filtering, washing with alcohol, pumping and drying.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a method for refining and crystallizing glucuronolactone. Background technique [0002] Glucuronolactone, also known as liver Tyler, glucuronolactone. The English name is D-Galacturonolactone, the molecular formula is C6H8O6, and the molecular weight is 176.12. Chemical properties: This product is white crystal or crystalline powder; odorless, slightly bitter taste; the color gradually becomes darker when exposed to light; after dissolving in water, part of the lactone becomes glucuronic acid, reaches an equilibrium state, and shows an acidic reaction. This product is easily soluble in water, slightly soluble in methanol and slightly soluble in ethanol. The melting point is 170-176°C (decomposition), and the specific rotation is +18.0°-+20.0° (0.1g / ml). The molecular structural formula is as follows: [0003] [0004] After this product enters the body, under the catalysis of the e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H7/033C07H1/06
Inventor 杨国军朱占元
Owner JIANGSU TASLY DIYI PHARMA CO LTD
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