Rectification and crystallization method of glucurolactone

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

Active Publication Date: 2014-11-05
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

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1. The refining method of the present invention

[0038] Mix 500kg of corn starch with 550kg of 75% nitric acid in the reactor, and add 10kg of sodium nitrite at the same time, and then react at 45℃ for 5 hours. After keeping warm, add water to dilute to an aqueous solution with an acid content of 8%, and transfer the aqueous solution to hydrolysis In the kettle, carry out hydrolysis under pressure at 0.25~0.28Mpa and about 135°C for 1 hour. After the hydrolysis is completed, the hydrolyzed solution is concentrated under vacuum at a temperature below 55°C to a concentration of about 45Be. The concentrated solution is mixed with glacial acetic acid 250kg at 45°C for esterification and kept for 16hrs. , And then concentrated the esterification solution, the concentrated esterification solution was cooled and crystallized for 3 days, and centrifuged to obtain 105 kg of crude glucurolactone.

[0039] Add 80 kg of purified water to the decolorization kettle, and add 10...

Embodiment 2

[0040] Example 2. The refining method of the present invention

[0041] Mix 500kg of corn starch with 550kg of 78% nitric acid in the reaction kettle, and add 10kg of sodium nitrite at the same time, then react at 45°C for 5 hours, after keeping warm, add water to dilute to an aqueous solution with an acid content of 8%, and transfer the aqueous solution to hydrolysis In the kettle, carry out hydrolysis under pressure at 0.25~0.28Mpa and 135°C for 1 hour. After the hydrolysis is completed, the hydrolyzate is concentrated in vacuo at a temperature below 55°C to a concentration of about 45Be. The concentrated solution is mixed with 250kg of glacial acetic acid at 45°C for esterification and kept for 15hrs. Then the esterification liquid was concentrated, and the concentrated esterification liquid was cooled and crystallized for 3 days, and centrifuged to obtain 108 kg of crude glucurolactone.

[0042] Add 100 kg of purified water to the decolorization kettle, and add 100 kg of powder...

Embodiment 3

[0043] Embodiment 3. The refining method of the present invention

[0044] Mix 500kg of corn starch with 550kg of 78% nitric acid in the reaction kettle, and add 10kg of sodium nitrite at the same time, and then react at 45°C for 5 hours. After heat preservation, add water to dilute to an aqueous solution with an acid content of 8%, and transfer the aqueous solution to hydrolysis In the kettle, carry out hydrolysis under pressure at 0.25~0.28Mpa and 138°C for 1 hour. After the hydrolysis is completed, the hydrolyzate is concentrated in vacuo at a temperature below 55°C to a concentration of about 45Be. The concentrated solution is mixed with 250kg of glacial acetic acid and esterified at 45°C, and kept for 16hrs. Then the esterification liquid was concentrated, and the concentrated esterification liquid was cooled and crystallized for 3 days, and centrifuged to obtain 106 kg of crude glucurolactone.

[0045] Add 80 kg of purified water to the decolorization kettle, and add 100 kg o...

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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 the refined crystallization of glucurolactone. Background technique [0002] Glucuronolactone is also known as liver Tyler and glucuronolactone. English name D-Galacturonolactone, molecular formula C6H8O6, molecular weight 176.12. Chemical properties: This product is white crystal or crystalline powder; odorless, slightly bitter taste; darker when exposed to light; after dissolving in water, part of the lactone turns into glucuronic acid, reaching an equilibrium state, showing an acidic reaction. This product is easily soluble in water, slightly soluble in methanol, 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 structure is as follows: [0003] [0004] After this product enters the body, under the catalysis of enzymes, the lactone ring is opened and becomes glucuronic acid to play...

Claims

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Application Information

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Patent Type & Authority Patents(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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