A kind of preparation method of d-glucosamine

Abstract

The invention relates to the field of chemistry, particularly to a D-glucosamine preparation method, wherein D-glucosamine hydrochloride is used as a raw material, ethanol with a concentration of 65-98% is used as a reaction solvent, an organic alkali is used as a deacidification agent, a solid-liquid exchange reaction is performed, the D-glucosamine maintains the solid-state form, the reaction solvent is removed through centrifugal separation, and soaking washing is performed with an ethanol solvent to obtain the high-purity D-glucosamine, wherein the obtained product has the low chlorine ioncontent and the high product purity. According to the present invention, the chlorine ion content determined by using the silver nitrate titration method (Volhard method) is less than 0.1%, such thatthe results indicate that the prepared D-glucosamine substantially does not contain sodium chloride and organic amine hydrochloride.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a preparation method of D-glucosamine. Background technique [0002] D-glucosamine, English name Glucosamine, chemical name: 2-amino-2-deoxy-D(+)-glucopyranose. (3R,4R,5S,6R)-3-Amino-6-(hydroxymethyl)oxane-2,4,5-triol. [0003] Chemical Structure: [0004] [0005] Molecular formula is C 6 h 13 o 5 N, CAS: 3416-24-8, molar mass 179.17g / mol. D-glucosamine is a compound in which one hydroxyl group of glucose is replaced by an amino group, commonly known as amino sugar, or ammonia sugar for short. Also known as glucosamine, widely present in nature, D-glucosamine is usually in the form of N-acetyl derivatives (such as chitin) or in the form of N-sulfate and N-acetyl-3-O-lactate ether (muramic acid) Exist in microorganisms, polysaccharides of animal origin and conjugated polysaccharides. D-glucosamine, which is a substance synthesized in the human body, is an important nutrient fo...

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Problems solved by technology

[0008] Chinese patent application CN 101899071A, in methanol or a mixed solvent of methanol and water, react alkalis such as sodium methoxide, sodium hydroxide or organic amine deacidification agents with D-glucosamine hydrochloride, and the D-glucosamine hydrochloride produced by the reaction will Dissolved in methanol or a mixed solvent of methanol and water, sodium methoxide, sodium hydroxide, etc. and chloride ions to form sodium chloride insoluble in solvents, after solid-liquid separation to remove the solid phase, then add a poor solvent of D-glucosamine to the solution , so that D-glucosamine is precipitated in solid form, the amount of solvent consumed by this method is relatively large, and the salt content of the product is relatively high

[0009] In the above-mentioned method of prior art, an obvious shortcoming is exactly that the use of methanol has certain toxicity, which has a greater impact on the health of workers, and the use of dehydrated alcohol requires secondary reactions, which are cumbersome to operate and cost too high; at the same time, the above-mentioned method ( In Chinese patent application CN 101899071A), sodium chloride or organic amine hydrochloride has certain solubility in methanol or methanol / water solvent, when adding organic solvent to the solution containing D-glucosamine to separate out D-glucosamine, these Substances are also precipitated at the same time, so what is often obtained is a mixture, and it is difficult to obtain high-purity D-glucosamine. The specific performance is that the content of chloride ions in the product is high, and the content of inorganic salts or organic salts is high, which often cannot meet the requirements of the drug. Product quality requirements for synthetic reactions or pharmaceutical health products

At the same time, in the above-mentioned patent method, the amount of solvent is large, the operation is complicated, and some examples also involve more toxic reagents.

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