CN106946954A - A kind of preparation method of N acetyl D Glucosamines - Google Patents
A kind of preparation method of N acetyl D Glucosamines Download PDFInfo
- Publication number
- CN106946954A CN106946954A CN201710197693.1A CN201710197693A CN106946954A CN 106946954 A CN106946954 A CN 106946954A CN 201710197693 A CN201710197693 A CN 201710197693A CN 106946954 A CN106946954 A CN 106946954A
- Authority
- CN
- China
- Prior art keywords
- acetylamino
- deoxy
- glucose
- glucosamines
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
- C07H5/04—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to nitrogen
- C07H5/06—Aminosugars
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Cosmetics (AREA)
Abstract
A kind of preparation method of N acetyl D Glucosamines, its step is as follows：D aminoglucose hydrochlorides raw material is reacted in a solvent with alkaline matter, free D Glucosamines are obtained；It is filtrated to get the solution containing free D Glucosamines；Add acetic anhydride and acetylation is carried out under conditions of 10 60 DEG C to D Glucosamines；The mixture of above-mentioned gained is filtered, obtained N acetyl D Glucosamines reprocessing obtains fine work N acetyl D Glucosamines, dries, that is, obtain finished product N acetyl D Glucosamines；The equipment that preparation method of the present invention needs is simple, it all can be used for preparing food, the common apparatus of medicine, the raw material of use, auxiliary material is all food, pharmaceutical production requirement, cheap, simple production process, production cost is low, the accessory substance of preparation process production is also that can be applied on food, and whole production process is easy to industrialization.
Description
Technical field
The present invention relates to a kind of preparation method of the saccharide compound containing acetylamino, especially a kind of N- acetyl-D-
The preparation method of Glucosamine.
Background technology
2-acetylamino-2-deoxy-D-glucose is newest third generation heath-function food additive in chitin health food series
Plus agent, had a wide range of applications in field of food.
2-acetylamino-2-deoxy-D-glucose is a kind of new food additives, is the base of a variety of important polysaccharide in organism
This component units, with important physiological function.2-acetylamino-2-deoxy-D-glucose can treat various inflammation, with enhancing people
The function of body immune system, is also the important as precursors for synthesizing bifidus factor and hyaluronic acid.In treatment tumour, tumour cell is prevented
Growth, reduces cholesterol, and reducing blood lipid, hypotensive is lost weight, and effect is notable in terms of increasing the absorption of calcium.Available for patient of diabetes
Person's sweetener, the antioxidant and infant food additive of food.Had a wide range of applications in terms of cosmetics.
The production method of 2-acetylamino-2-deoxy-D-glucose has organic chemistry method, fermentation method, enzymatic isolation method.Organic chemistry method by
In applying poisonous and hazardous organic matter in preparation process, due to residual venomous injurant so that product can not be answered in food
With., due to microbe, there are many uncertain factors in preparation process in fermentation method and enzymatic isolation method, can generate it is other not
Impurity is known, so as to be restricted in field of food.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of new N- acetyl-D- ammonia in view of the shortcomings of the prior art
The preparation method of base glucose, obtained 2-acetylamino-2-deoxy-D-glucose purity is high, technique is simple, easy to operate, is adapted to extensive
Production.
The technical problems to be solved by the invention are realized by following technical scheme.The present invention is a kind of N- second
The preparation method of acyl-D- Glucosamines, comprises the following steps：
（1）It is free：D-Glucosamine Hydrochloride raw material is reacted in a solvent with alkaline matter first, D- glucosamine salts
The mol ratio of hydrochlorate raw material and alkaline matter is 1:0.5-6, obtains free D- Glucosamines；D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is preferably 1:1-5, more preferably 1:2-3；
（2）Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- amino
Glucose solution；
（3）Acetylation：Add acetic anhydride and carry out acetylation, D- amino Portugal under conditions of -10 DEG C -60 DEG C to D- Glucosamines
The mol ratio of grape sugar hydrochloride Starting material and acetic anhydride is 1:0.8-10；The temperature conditionss of acetylation are preferably -5 DEG C -30 DEG C, enter one
Step is preferably 0 DEG C -25 DEG C, is further preferably 5 DEG C -20 DEG C；The mol ratio of D-Glucosamine Hydrochloride raw material and acetic anhydride is preferred
For 1:1-7, more preferably 1:2-5, is further preferably 1：3-4；
（4）Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D- ammonia
Base glucose is reprocessed, and obtains fine work 2-acetylamino-2-deoxy-D-glucose, is dried, you can obtain finished product N- acetyl-D-amino grapes
Sugar；
The preparation method of 2-acetylamino-2-deoxy-D-glucose of the present invention avoids using tri-n-butylamine, triethylamine, and sodium methoxide etc. is poisonous to be had
Harmful organic solvent, used raw material and auxiliary material are all food-grade or pharmaceutical grade, and preparation process, which will not be brought, any poisonous to be had
Harmful accessory substance, whole preparation process is simple to operate, and technique is advanced, without any pollution, is truly realized clean manufacturing, gained
2-acetylamino-2-deoxy-D-glucose no matter outward appearance, or inherent quality is really achieved food-grade, pharmaceutical grade requirement.
The equipment that the preparation method of 2-acetylamino-2-deoxy-D-glucose of the present invention needs is simple, all can be used for preparing food
Product, the common apparatus of medicine, the raw material of use, auxiliary material is all food, and pharmaceutical production is required, cheap, simple production process,
Production cost is low, and the accessory substance of preparation process production is also that can be applied on food, and whole production process is easy to industry
Change.
Embodiment
Concrete technical scheme of the invention described further below, in order to which those skilled in the art can be best understood from
The present invention, without constituting the limitation to its right.
Embodiment 1.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water first, D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is 1:0.5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of -10 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:0.8；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 2.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material is reacted in ethanol with alkaline matter first, D- glucosamine hydrochloric acids
The mol ratio of salt raw material and alkaline matter is 1:1, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of -5 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:1；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 3.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water and alcohol mixed solution first, D- ammonia
The mol ratio of base glucosamine salt hydrochlorate raw material and alkaline matter is 1:2, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and acetylation, D-Glucosamine Hydrochloride are carried out under conditions of 0 DEG C to D- Glucosamines
The mol ratio of raw material and acetic anhydride is 1:3；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 4.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water first, D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is 1:6, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and acetylation, D-Glucosamine Hydrochloride are carried out under conditions of 5 DEG C to D- Glucosamines
The mol ratio of raw material and acetic anhydride is 1:4；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 5.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material is reacted in ethanol with alkaline matter first, D- glucosamine hydrochloric acids
The mol ratio of salt raw material and alkaline matter is 1:5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 10 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:5；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 6.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water and alcohol mixed solution first, D- ammonia
The mol ratio of base glucosamine salt hydrochlorate raw material and alkaline matter is 1:4, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 20 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:10；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 7.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water first, D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is 1:3, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 60 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:8；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 8.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material is reacted in ethanol with alkaline matter first, D- glucosamine hydrochloric acids
The mol ratio of salt raw material and alkaline matter is 1:2, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 30 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:2；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 9.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water and alcohol mixed solution first, D- ammonia
The mol ratio of base glucosamine salt hydrochlorate raw material and alkaline matter is 1:2, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 40 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:5；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 10.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water first, D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is 1:1, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 25 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:2；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 11.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material is reacted in ethanol with alkaline matter first, D- glucosamine hydrochloric acids
The mol ratio of salt raw material and alkaline matter is 1:5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 45 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:1.5；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 12.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water and alcohol mixed solution first, D- ammonia
The mol ratio of base glucosamine salt hydrochlorate raw material and alkaline matter is 1:2.5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 15 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:1.2；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 13.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water first, D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is 1:3, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of -5 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:10；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 14.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material is reacted in ethanol with alkaline matter first, D- glucosamine hydrochloric acids
The mol ratio of salt raw material and alkaline matter is 1:3, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of -5 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:9；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 15.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water and alcohol mixed solution first, D- ammonia
The mol ratio of base glucosamine salt hydrochlorate raw material and alkaline matter is 1:0.5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of -10 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:10；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 16.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water first, D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is 1:3.5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 10 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:7；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 17.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material is reacted in ethanol with alkaline matter first, D- glucosamine hydrochloric acids
The mol ratio of salt raw material and alkaline matter is 1:3.8, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of -1 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:5；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 18.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water and alcohol mixed solution first, D- ammonia
The mol ratio of base glucosamine salt hydrochlorate raw material and alkaline matter is 1:3, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 20 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:5；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 19.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water first, D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is 1:1.5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 40 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:5.5；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 20.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material is reacted in ethanol with alkaline matter first, D- glucosamine hydrochloric acids
The mol ratio of salt raw material and alkaline matter is 1:4.5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 35 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:2；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 21.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water and alcohol mixed solution first, D- ammonia
The mol ratio of base glucosamine salt hydrochlorate raw material and alkaline matter is 1:1.5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 25 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:7.5；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 22.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water first, D-Glucosamine Hydrochloride
The mol ratio of raw material and alkaline matter is 1:6, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 60 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:10；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 23.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material is reacted in ethanol with alkaline matter first, D- glucosamine hydrochloric acids
The mol ratio of salt raw material and alkaline matter is 1:0.8, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 25 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:2；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
Embodiment 24.A kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, its step is as follows：
It is free：D-Glucosamine Hydrochloride raw material and alkaline matter are reacted in water and alcohol mixed solution first, D- ammonia
The mol ratio of base glucosamine salt hydrochlorate raw material and alkaline matter is 1:4.5, obtain free D- Glucosamines；
Ultrafiltration：The solution of above-mentioned gained is filtered, the material such as insoluble matter and bacterium is removed, obtained containing free D- aminoglucoses
Sugar juice；
Acetylation：Add acetic anhydride and carry out acetylation, D- glucosamine hydrochloric acids under conditions of 35 DEG C to D- Glucosamines
The mol ratio of salt raw material and acetic anhydride is 1:2.5；
Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D-aminos Portugal
Grape sugar reprocessing, obtains fine work 2-acetylamino-2-deoxy-D-glucose, dries, you can obtain finished product 2-acetylamino-2-deoxy-D-glucose.
In above-described embodiment, alkaline matter is selected from the material of sodium, potassium, calcium, the alkaline matter of magnesium and ammonia.The thing of described ammonia
Matter is selected from the ethanol solution of ammonia, ammoniacal liquor or ammonia.The alkaline matter of sodium is selected from sodium acetate, NaOH, sodium carbonate, bicarbonate
Sodium, sodium phosphate, sodium dihydrogen phosphate or disodium hydrogen phosphate.The alkaline matter of potassium is selected from potassium acetate, potassium hydroxide, potassium carbonate, carbon
Potassium hydrogen phthalate, potassium phosphate, potassium dihydrogen phosphate or dipotassium hydrogen phosphate.The alkaline matter of calcium be calcium acetate, calcium hydroxide, calcium carbonate or
Person's calcium bicarbonate；The alkaline matter of magnesium is selected from magnesium acetate, magnesium hydroxide, magnesium carbonate or magnesium bicarbonate.Ultrafiltration is selected from micropore mistake
Filter, filter paper filtering, filter-cloth filtering, deckle board filtering or centrifugal filtration.Reprocessing selected from washing, crystal's system, ethanol wash, water and
Alcohol mixture is refined or water and alcohol mixture washing.
Dry selected from vacuum drying, drying or be spray-dried.
Claims (10)
1. a kind of preparation method of 2-acetylamino-2-deoxy-D-glucose, it is characterised in that characterized in that, its step is as follows：
（1）It is free：D-Glucosamine Hydrochloride raw material is reacted in a solvent with alkaline matter first, D- glucosamine salts
The mol ratio of hydrochlorate raw material and alkaline matter is 1:0.5-6, obtains free D- Glucosamines；
（2）Ultrafiltration：The solution of above-mentioned gained is filtered, insoluble matter and bacterium is removed, obtained containing free D- Glucosamines
Solution；
（3）Acetylation：Add acetic anhydride and carry out acetylation, D- aminoglucoses under conditions of -10-60 DEG C to D- Glucosamines
The mol ratio of sugared hydrochloride Starting material and acetic anhydride is 1:0.8-10；
（4）Filtering：The mixture of above-mentioned gained is filtered, 2-acetylamino-2-deoxy-D-glucose is obtained；Obtained N- acetyl-D- ammonia
Base glucose is reprocessed, and obtains fine work 2-acetylamino-2-deoxy-D-glucose, is dried, that is, is obtained finished product N- acetyl-D-amino grapes
Sugar.
2. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 1, it is characterised in that：Step（1）In
Alkaline matter is selected from the material of sodium, potassium, calcium, the alkaline matter of magnesium and ammonia.
3. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 2, it is characterised in that：Described ammonia
Material is the ethanol solution of ammonia, ammoniacal liquor or ammonia.
4. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 2, it is characterised in that：The basic species of sodium
Matter is selected from sodium acetate, NaOH, sodium carbonate, sodium acid carbonate, sodium phosphate, sodium dihydrogen phosphate or disodium hydrogen phosphate.
5. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 2, it is characterised in that：The basic species of potassium
Matter is selected from potassium acetate, potassium hydroxide, potassium carbonate, saleratus, potassium phosphate, potassium dihydrogen phosphate or dipotassium hydrogen phosphate.
6. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 2, it is characterised in that：The basic species of calcium
Matter is calcium acetate, calcium hydroxide, calcium carbonate or calcium bicarbonate；The alkaline matter of magnesium is selected from magnesium acetate, magnesium hydroxide, magnesium carbonate
Or magnesium bicarbonate.
7. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 1, it is characterised in that：Step（1）In
Solvent is selected from the mixture of water, ethanol or water and ethanol.
8. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 1, it is characterised in that：Step（2）It is described
Ultrafiltration be selected from micro porous filtration, filter paper filtering, filter-cloth filtering, deckle board filter or centrifugal filtration.
9. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 1, it is characterised in that：Step（4）Middle institute
The reprocessing stated is selected from washing, the washing of crystal's system, ethanol, water and alcohol mixture and refined or water and alcohol mixture washing.
10. the preparation method of 2-acetylamino-2-deoxy-D-glucose according to claim 1, it is characterised in that：Step（4）Institute
The drying stated is selected from vacuum drying, drying or is spray-dried.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710197693.1A CN106946954A (en) | 2017-03-29 | 2017-03-29 | A kind of preparation method of N acetyl D Glucosamines |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710197693.1A CN106946954A (en) | 2017-03-29 | 2017-03-29 | A kind of preparation method of N acetyl D Glucosamines |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106946954A true CN106946954A (en) | 2017-07-14 |
Family
ID=59475437
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710197693.1A Pending CN106946954A (en) | 2017-03-29 | 2017-03-29 | A kind of preparation method of N acetyl D Glucosamines |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106946954A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669082A (en) * | 2019-10-23 | 2020-01-10 | 山东润德生物科技有限公司 | Purification and separation method of N-acetyl-D-glucosamine |
| CN110684057A (en) * | 2019-11-22 | 2020-01-14 | 山东润德生物科技有限公司 | Production method of N-acetyl-D-glucosamine |
| CN110845552A (en) * | 2019-11-22 | 2020-02-28 | 山东润德生物科技有限公司 | Preparation method of acylated derivative of glucosamine |
| CN111574230A (en) * | 2020-05-15 | 2020-08-25 | 湖北亿纬动力有限公司 | Modified nano ceramic particles and preparation method thereof, ceramic diaphragm slurry and preparation method thereof, diaphragm and lithium ion battery |
| CN115448963A (en) * | 2022-10-21 | 2022-12-09 | 扬州日兴生物科技股份有限公司 | Preparation method of N-acetyl-D-glucosamine |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1907993A (en) * | 2006-08-22 | 2007-02-07 | 王松叶 | Process for preparing refined N-acetyl-D-aminoglucose |
| CN101830938A (en) * | 2010-05-19 | 2010-09-15 | 王松叶 | Preparation method of N-acetyl-D-glucosamine |
| CN105753913A (en) * | 2016-02-04 | 2016-07-13 | 厦门蓝湾科技有限公司 | Preparation method of high-purity N-acetyl-D-glucosamine |
| CN106008615A (en) * | 2016-06-01 | 2016-10-12 | 江苏澳新生物工程有限公司 | Method for preparing N-acetyl-D-glucosamine from chitin |
-
2017
- 2017-03-29 CN CN201710197693.1A patent/CN106946954A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1907993A (en) * | 2006-08-22 | 2007-02-07 | 王松叶 | Process for preparing refined N-acetyl-D-aminoglucose |
| CN101830938A (en) * | 2010-05-19 | 2010-09-15 | 王松叶 | Preparation method of N-acetyl-D-glucosamine |
| CN105753913A (en) * | 2016-02-04 | 2016-07-13 | 厦门蓝湾科技有限公司 | Preparation method of high-purity N-acetyl-D-glucosamine |
| CN106008615A (en) * | 2016-06-01 | 2016-10-12 | 江苏澳新生物工程有限公司 | Method for preparing N-acetyl-D-glucosamine from chitin |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669082A (en) * | 2019-10-23 | 2020-01-10 | 山东润德生物科技有限公司 | Purification and separation method of N-acetyl-D-glucosamine |
| CN110684057A (en) * | 2019-11-22 | 2020-01-14 | 山东润德生物科技有限公司 | Production method of N-acetyl-D-glucosamine |
| CN110845552A (en) * | 2019-11-22 | 2020-02-28 | 山东润德生物科技有限公司 | Preparation method of acylated derivative of glucosamine |
| CN111574230A (en) * | 2020-05-15 | 2020-08-25 | 湖北亿纬动力有限公司 | Modified nano ceramic particles and preparation method thereof, ceramic diaphragm slurry and preparation method thereof, diaphragm and lithium ion battery |
| CN115448963A (en) * | 2022-10-21 | 2022-12-09 | 扬州日兴生物科技股份有限公司 | Preparation method of N-acetyl-D-glucosamine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106946954A (en) | A kind of preparation method of N acetyl D Glucosamines | |
| CN110669081B (en) | Method for preparing glucosamine sulfate | |
| KR101915730B1 (en) | Method for manufacturing High Purity Chitosan, and The Chitosan produced Thereby | |
| CN111018926B (en) | Method for extracting high-purity glucosamine hydrochloride from glucosamine fermentation broth | |
| CN110804108B (en) | Preparation method of water-soluble alginate for in vivo implantation | |
| CN110734465B (en) | Preparation method of glucosamine potassium sulfate salt | |
| CN107325205A (en) | A kind of inulin and FOS syrup co-production | |
| CN101492408A (en) | Method for separating tryptophane from fermentation liquor | |
| JP2004269663A (en) | Method for purifying crocetin | |
| CN109265498A (en) | A kind of method that integrated poly sialic acid separating-purifying prepares N-acetyl-neuraminate | |
| CN110804077A (en) | Preparation method of glucosamine hydrochloride | |
| CN110818751B (en) | Preparation method of glucosamine sulfate sodium chloride double salt | |
| US8383808B2 (en) | Method to prepare D-glucosamine hydrochloride | |
| JPH0586399B2 (en) | ||
| CN110862426A (en) | Method for preparing high-purity glucosamine sulfate | |
| CN102827306A (en) | Method for preparing pectin from capsicum residue | |
| CN104610385B (en) | A kind of process for purification of aminoglucose hydrochloride | |
| CA1092603A (en) | Process for preparing hydroxyethyl starch suitable as plasma expander | |
| CN110684057A (en) | Production method of N-acetyl-D-glucosamine | |
| JP6275341B2 (en) | Single-stranded β-glucan composition, method for producing the same, and liquid composition | |
| CN103360319A (en) | Method for producing histidine by taking amino acid I mother solution as raw material | |
| KR100688075B1 (en) | Process for preparing water soluble soy oligo-saccharide powder | |
| KR100834518B1 (en) | Method for preparing glucosamine organic acid with improved taste by an enzymatic process | |
| CN110590870B (en) | Preparation method of high-purity N-acetylglucosamine | |
| CN110606864B (en) | N-acetylneuraminic acid calcium salt crystal and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170714 |