CN112062694A - Preparation process of N-carbamylglutamic acid - Google Patents
Preparation process of N-carbamylglutamic acid Download PDFInfo
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- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/18—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas
- C07C273/1809—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas with formation of the N-C(O)-N moiety
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- C07C273/18—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas
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Abstract
The invention discloses a preparation process of N-carbamylglutamic acid. The invention relates to the technical field of biochemical materials. The preparation method comprises glutamic acid, urea, a catalyst, concentrated hydrochloric acid, distilled water and a plurality of reaction tools, and the preparation efficiency of the N-carbamylglutamic acid is gradually improved by arranging a reaction box with a heating device, an electric heating sleeve, a vacuum drying box, a circulating water vacuum pump, an ultra-low temperature refrigerator, a pulverizer, an electronic balance, a PH meter, a centrifugal machine, a high-power electric stirrer, an ultrapure water system and other components, so that the preparation efficiency of the N-carbamylglutamic acid is greatly improved, the industrial large-scale processing can be further adapted, and the cost for preparing the N-carbamylglutamic acid is reduced.
Description
Technical Field
The invention relates to the technical field of biochemical materials, in particular to a preparation process of N-carbamylglutamic acid.
Background
The Chinese name of NCG is: n-carbamylglutamic acid. The molecular formula is C6H10N2O5, the molecular weight is 190.15, and the pure product is colorless transparent crystal. NCG is insoluble in water and slightly soluble in organic solvent, the isoelectric point of the active substance is 3.02, and the salts thereof are soluble in water. By promoting the endogenous synthesis of arginine, the litter size and birth weight of animals are improved, the fertility of male animals is enhanced, and the growth and development of young animals are promoted.
NCG is N-acetyl glutamic acid (NAG) analogue, can play a role like NAG in the animal body to participate in the urea circulation of the body, has long half life, is stable in metabolism and has wide biological functions. Research shows that NCG can be used as a metabolism activator to participate in the activation of dihydropyrrole-5-carboxylic acid synthetase (P5CS) and carbamyl phosphate synthetase I (CPS-I), promotes the synthesis of citrulline and arginine from glutamine or proline, and is also called as an arginine endogenous activator. Nitric Oxide (NO) and polyamines have a wide range of actions in the body and can promote local blood circulation, arginine is indispensable as an essential precursor for synthesizing them, and NCG can effectively increase the content of arginine and is very important for maintaining arginine level and normal physiological functions of the body.
The solubility of N-carbamylglutamic acid in water increases along with the temperature rise, and the N-carbamylglutamic acid is slightly soluble in organic solvents such as ethanol, acetone and the like. The chemistry of N-carbamoylglutamic acid is mainly focused on the carboxyl group and the carbamoyl group at C2. The nucleophilic ability of amino group is strongest under alkaline and weak acidic condition, carboxyl group on C1 and C5 can generate acyl chloride with oxalyl chloride, acetyl chloride, PCL5 and the like under strong alkaline condition, and the chemical property of the compound is determined by the existence of a plurality of active groups.
N-carbamylglutamic acid is named as arginine biotin, in recent years, a significant discovery in the field of pig nutrition is that arginine amino acid plays an important role in regulating and controlling the nutrition metabolism and immune response of organisms, the mechanism and the effect are very clear, and scholars at home and abroad have reviewed the arginine amino acid, but because the cost of arginine is relatively high, the arginine is possibly interfered with the metabolism of other amino acids when being added according to effective dose in daily ration, so that the industry hopes to achieve the purposes of improving the arginine content of the organisms and improving the production and health of animals by another substance of arginine endogenous activator namely NCG.
At present, glutamic acid and potassium cyanate are generally used as raw materials, urea propionic acid is used as a catalyst, and a target compound N-carbamylglutamic acid is obtained through nucleophilic addition reaction and recrystallization purification.
Therefore, a preparation process of N-carbamylglutamic acid is provided to solve the problems.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation process of N-carbamylglutamic acid.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for preparing N-carbamylglutamic acid comprises preparing glutamic acid; 8-10 parts of urea: 2-4 parts; potassium hydroxide: 5-7 parts; catalyst: 2-3 parts of a solvent; concentrated hydrochloric acid: 1-2 parts; distilled water: 2-3 parts and a plurality of reaction tools.
Preferably, the reaction tool is selected from a reaction box with a heating device, an electric heating jacket, a vacuum drying box, a circulating water vacuum pump, an ultra-low temperature refrigerator, a pulverizer, an electronic balance, a PH meter, a centrifuge, a high-power electric stirrer and an ultra-pure water system.
Preferably, the method comprises the following steps: weighing the raw materials in parts by weight;
(1) firstly, sequentially adding glutamic acid, urea, potassium hydroxide and a catalyst into a reaction box of a heating device according to a proportion by an electronic balance, then adding water in a corresponding proportion, fully mixing the internal raw materials by a high-power electric stirrer, then opening the heating device to dissolve the solid, and controlling the temperature to be 60-65 ℃;
(2) after reacting for 2 hours, standing for 16-20 hours at room temperature, acidifying with concentrated hydrochloric acid, testing by a PH meter to ensure that the pH value is 6, standing for 2-3 hours, centrifuging and filtering by a centrifuge, and washing with water to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) and drying to obtain 20.8g of fine product. The yield was 87%, the content was 9%.
Preferably, the outer side of the heating reaction box can be sleeved with an electric heating sleeve, and the electric heating sleeve controls the temperature of the reaction box to be rapidly and stably 60-65 ℃.
Preferably, the solution in the reaction chamber of the heating device may be allowed to stand in an ultra-low temperature refrigerator.
Preferably, the crude product after centrifugal filtration by the centrifuge is dried by a vacuum drying oven.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts processing equipment with larger volume to improve the preparation quantity of the N-carbamylglutamic acid, and simultaneously, the preparation efficiency of the N-carbamylglutamic acid is gradually improved by arranging the reaction box with a heating device, the electric heating jacket, the vacuum drying box, the circulating water vacuum pump, the ultra-low temperature refrigerator, the pulverizer, the electronic balance, the PH meter, the centrifuge, the high-power electric stirrer, the ultrapure water system and other components, so that the preparation efficiency of the N-carbamylglutamic acid is greatly improved, the industrial large-scale processing can be further adapted, and the cost for preparing the N-carbamylglutamic acid is reduced.
Detailed Description
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated for convenience in describing the present invention and to simplify description, but do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be considered as limiting. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art from the specific situation
The technical solutions of the present invention are described in detail below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
(1) a worker uses an electronic balance to weigh 8 parts of glutamic acid, 2 parts of urea, 5 parts of potassium hydroxide and 2 parts of catalyst according to the proportion, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device is started to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in a reaction box of a heating device for 16-20 hours at room temperature, acidifying the solution by using concentrated hydrochloric acid, testing by using a PH meter to ensure that the pH value is 6, standing for 2-3 hours, performing centrifugal filtration by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering; and (4) drying the crystals obtained in the step (3) and drying to obtain fine products.
Example 2:
(1) a worker uses an electronic balance to weigh 8 parts of glutamic acid, 2 parts of urea, 5 parts of potassium hydroxide and 2 parts of catalyst according to the proportion, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device sleeved with an electric heating sleeve is opened to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in a reaction box of a heating device for 16-20 hours at room temperature, acidifying the solution by using concentrated hydrochloric acid, testing by using a PH meter to ensure that the pH value is 6, standing for 2-3 hours, performing centrifugal filtration by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) and drying to obtain fine products.
Thus, the temperature of the reaction box is controlled to be 60-65 ℃ rapidly and stably by the electric heating jacket, so that the heating and preheating time in large-scale production is increased, and the production efficiency of products is improved;
example 3:
(1) a worker uses an electronic balance to weigh 8 parts of glutamic acid, 2 parts of urea, 5 parts of potassium hydroxide and 2 parts of catalyst according to the proportion, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device is started to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in the reaction box of the heating device in an ultra-low temperature refrigerator for a period of time, then acidifying the solution by using concentrated hydrochloric acid, testing the pH value by using a pH meter to enable the pH value to be 6, standing the solution for 1 to 2 hours, centrifuging and filtering the solution by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) and drying to obtain fine products.
The crystallization efficiency of the solution is improved through the ultra-low temperature refrigerator, and the time required for standing is reduced, so that the production efficiency of the product is improved.
Example 4:
(1) a worker uses an electronic balance to weigh 8 parts of glutamic acid, 2 parts of urea, 5 parts of potassium hydroxide and 2 parts of catalyst according to the proportion, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device is started to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in a reaction box of a heating device for 16-20 hours at room temperature, acidifying the solution by using concentrated hydrochloric acid, testing by using a PH meter to ensure that the pH value is 6, standing for 2-3 hours, performing centrifugal filtration by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) through a vacuum drying oven, and drying to obtain fine products. Therefore, the time required by drying is reduced through the vacuum drying box, the drying efficiency is improved, and the production efficiency of products is improved to a certain extent.
Example 5:
(1) a worker uses an electronic balance to weigh according to the proportion of 10 parts of glutamic acid, 4 parts of urea, 7 parts of potassium hydroxide and 3 parts of catalyst, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device is started to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in a reaction box of a heating device for 16-20 hours at room temperature, acidifying the solution by using 1 part of concentrated hydrochloric acid, testing by using a pH meter to ensure that the pH value is 6, standing for 2-3 hours, centrifuging and filtering the solution by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) and drying to obtain fine products.
Thus, the quantity of finished products prepared after reaction is increased by increasing the weight of materials, and the production efficiency of the products is improved on the other hand.
Example 6:
(1) a worker uses an electronic balance to weigh 8 parts of glutamic acid, 2 parts of urea, 5 parts of potassium hydroxide and 2 parts of catalyst according to the proportion, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device is started to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(1) after reacting for 2 hours, standing the solution in a reaction box of a heating device for 16-20 hours at room temperature, acidifying the solution by using concentrated hydrochloric acid, testing by using a PH meter to ensure that the pH value is 6, standing for 2-3 hours, performing centrifugal filtration by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, filtering, and then treating the water after reaction by using a circulating water vacuum pump for mixing in the initial product production;
(4) and (4) drying the crystals obtained in the step (3) through a vacuum drying oven, and drying to obtain fine products. The waste of water resources can be reduced through the circulating water vacuum pump, so that the energy is saved, the environment is protected, the production cost can be saved, the product price is reduced, and the market advantage is obtained.
Example 7:
(1) a worker uses an electronic balance to weigh 8 parts of glutamic acid, 2 parts of urea, 5 parts of potassium hydroxide and 2 parts of catalyst according to the proportion, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device sleeved with an electric heating sleeve is opened to dissolve solids, and the temperature is controlled to be 60-65 ℃;
after reacting for 2 hours, standing the solution in the reaction box of the heating device in an ultra-low temperature refrigerator for a period of time, then acidifying the solution by using concentrated hydrochloric acid, testing the pH value by using a pH meter to be 6, standing the solution for 2 to 3 hours, then performing centrifugal filtration by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering; then the water after reaction is treated by a circulating water vacuum pump and is used for the initial product production and mixing.
(4) And (4) drying the crystals obtained in the step (3) through a vacuum drying oven, and drying to obtain fine products. By processing the equipment in a centralized manner, the production efficiency of the product is improved from each process link of the processing, and meanwhile, the produced cost is reduced, so that the quantity of the prepared products is increased and the production cost is reduced.
Example 8:
(1) a worker uses an electronic balance to weigh according to the proportion of 10 parts of glutamic acid, 4 parts of urea, 7 parts of potassium hydroxide and 3 parts of catalyst, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device sleeved with an electric heating sleeve is opened to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in a reaction box of a heating device for 16-20 hours at room temperature, acidifying the solution by using 1 part of concentrated hydrochloric acid, testing by using a pH meter to ensure that the pH value is 6, standing for 2-3 hours, centrifuging and filtering the solution by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) and drying to obtain fine products.
Thus, the quantity of the finished products prepared after reaction is increased by increasing the weight of the materials and controlling the heating speed and the temperature area, thereby improving the production efficiency of the products on the other hand;
example 9:
(1) a worker uses an electronic balance to weigh according to the proportion of 10 parts of glutamic acid, 4 parts of urea, 7 parts of potassium hydroxide and 3 parts of catalyst, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device is started to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in the reaction box of the heating device in an ultra-low temperature refrigerator for a period of time, then acidifying the solution by using concentrated hydrochloric acid, testing the pH value by using a pH meter to enable the pH value to be 6, standing the solution for 1 to 2 hours, centrifuging and filtering the solution by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) and drying to obtain fine products.
Thus, the quantity of the materials is increased and the standing crystallization time is reduced, so that the quantity of finished products prepared after reaction is increased, and the production efficiency of the products is improved.
Example 10:
(1) a worker uses an electronic balance to weigh according to the proportion of 10 parts of glutamic acid, 4 parts of urea, 7 parts of potassium hydroxide and 3 parts of catalyst, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device is started to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in a reaction box of a heating device for 16-20 hours at room temperature, acidifying the solution by using 1 part of concentrated hydrochloric acid, testing by using a pH meter to ensure that the pH value is 6, standing for 2-3 hours, centrifuging and filtering the solution by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) through a vacuum drying oven, and drying to obtain fine products. The quantity of finished products is increased by increasing the weight of materials and improving the drying time of fine products, and the production efficiency of the products is also improved.
Example 11:
1) a worker uses an electronic balance to weigh according to the proportion of 10 parts of glutamic acid, 4 parts of urea, 7 parts of potassium hydroxide and 3 parts of catalyst, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device is started to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in a reaction box of a heating device for 16-20 hours at room temperature, acidifying the solution by using 1 part of concentrated hydrochloric acid, testing by using a pH meter to ensure that the pH value is 6, standing for 2-3 hours, centrifuging and filtering the solution by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, filtering, and then treating the water after reaction by using a circulating water vacuum pump for mixing in the initial product production;
(4) and (4) drying the crystals obtained in the step (3) and drying to obtain fine products.
Thus, the quantity of the materials is increased and the process cost is reduced, so that the quantity of finished products prepared after reaction is increased, the production efficiency of the products is improved and the production cost is reduced.
Example 12:
(1) a worker uses an electronic balance to weigh according to the proportion of 10 parts of glutamic acid, 4 parts of urea, 7 parts of potassium hydroxide and 3 parts of catalyst, then the glutamic acid, the urea, the potassium hydroxide and the catalyst are sequentially added into a reaction box of a heating device according to the proportion, water which is treated by an ultrapure water system according to the corresponding proportion is added, internal raw materials are fully mixed through a high-power electric stirrer, then the heating device sleeved with an electric heating sleeve is opened to dissolve solids, and the temperature is controlled to be 60-65 ℃;
(2) after reacting for 2 hours, standing the solution in the reaction box of the heating device in an ultra-low temperature refrigerator for a period of time, then acidifying the solution by using concentrated hydrochloric acid, testing the pH value by using a pH meter to enable the pH value to be 6, standing the solution for 1 to 2 hours, centrifuging and filtering the solution by using a centrifugal machine, and washing the solution to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, filtering, and then treating the water after reaction by using a circulating water vacuum pump for mixing in the initial product production;
(4) and (4) drying the crystals obtained in the step (3) through a vacuum drying oven, and drying to obtain fine products. By improving the efficiency and reducing the cost in an all-round way, the number of the manufactured products is increased, the production cost is reduced, the market competitiveness of the products is favorably improved, and the large-scale production of enterprises is facilitated.
The invention adopts processing equipment with larger volume and raw material quantity with different proportions to improve the preparation quantity of the N-carbamylglutamic acid, comprising a plurality of glutamic acid parts, urea, catalysts, concentrated hydrochloric acid, distilled water and reaction tools, and is matched with a reaction box with a heating device, an electric heating jacket, a vacuum drying box, a circulating water vacuum pump, an ultra-low temperature refrigerator, a pulverizer, an electronic balance, a PH meter, a centrifuge, a high-power electric stirrer, an ultrapure water system and other components to gradually improve the preparation efficiency of the N-carbamylglutamic acid, greatly improve the preparation efficiency of the N-carbamylglutamic acid, reduce the time cost and the material cost in the process, and ensure that the generated process is more energy-saving and environment-friendly by the circulating water vacuum pump, thereby responding to national calls and further adapting to factory large-scale processing, the cost for preparing the N-carbamylglutamic acid is reduced, and the market competitiveness of the product is improved, thereby facilitating the large-scale production of enterprises.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may include only a single embodiment, and such description is for clarity only, and those skilled in the art will be able to make the description as a whole, and the embodiments may be appropriately combined to form other embodiments as will be apparent to those skilled in the art.
Claims (6)
1. A process for preparing N-carbamylglutamic acid comprises preparing glutamic acid; 8-10 parts of urea: 2-4 parts; potassium hydroxide: 5-7 parts; catalyst: 2-3 parts of a solvent; concentrated hydrochloric acid: 1-2 parts; distilled water: 2-3 parts and a plurality of reaction tools.
2. The process for preparing N-carbamylglutamic acid according to claim 1, wherein the reaction tool is selected from a reaction tank with a heating device, an electric heating jacket, a vacuum drying tank, a circulating water vacuum pump, an ultra-low temperature refrigerator, a pulverizer, an electronic balance, a pH meter, a centrifuge, a high-power electric stirrer and an ultra-pure water system.
3. The process for preparing N-carbamylglutamic acid according to claims 1-2, characterized by comprising the following steps: weighing the raw materials in parts by weight;
(1) firstly, sequentially adding glutamic acid, urea, potassium hydroxide and a catalyst into a reaction box of a heating device according to a proportion by an electronic balance, then adding water in a corresponding proportion, fully mixing the internal raw materials by a high-power electric stirrer, then opening the heating device to dissolve the solid, and controlling the temperature to be 60-65 ℃;
(2) after reacting for 2 hours, standing for 16-20 hours at room temperature, acidifying with concentrated hydrochloric acid, testing by a PH meter to ensure that the pH value is 6, standing for 2-3 hours, centrifuging and filtering by a centrifuge, and washing with water to be neutral to obtain a crude product;
(3) recrystallizing the crude product in the step (2) by water provided by an ultrapure water system, and then filtering;
(4) and (4) drying the crystals obtained in the step (3) and drying to obtain 20.8g of fine product. The yield was 87%, the content was 9%.
4. The process for preparing N-carbamylglutamic acid according to claims 1 to 3, wherein the outside of the heating reaction chamber can be sleeved with an electric heating jacket, and the electric heating jacket controls the temperature of the reaction chamber to be rapidly and stably 60 to 65 ℃.
5. The process for preparing N-carbamylglutamic acid according to claims 1 to 3, wherein the solution in the reaction tank of the heating device can be left to stand in an ultra-low temperature refrigerator.
6. The process for preparing N-carbamylglutamic acid according to claims 1-3, characterized in that the crude product after centrifugal filtration by the centrifuge is dried by a vacuum drying oven.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168518A (en) * | 2007-11-13 | 2008-04-30 | 印遇龙 | Method for preparing N-carbamyl glutamic acid |
| CN101481336A (en) * | 2009-01-19 | 2009-07-15 | 南昌大学 | Preparation of N-carbamoyl-aminoglutaric acid and sodium salt thereof |
| CN103980163A (en) * | 2014-05-30 | 2014-08-13 | 南京工业大学 | Method for continuously synthesizing N-carbamylglutamic acid by using microchannel reactor |
| CN105601542A (en) * | 2016-01-08 | 2016-05-25 | 南京工业大学 | Method for crystallizing N-carbamylglutamic acid by using mixed acid |
| CN108484448A (en) * | 2018-04-27 | 2018-09-04 | 湖北泓肽生物科技有限公司 | The method of one pot process N- carbamylglutamic acids |
-
2020
- 2020-08-07 CN CN202010786638.8A patent/CN112062694A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168518A (en) * | 2007-11-13 | 2008-04-30 | 印遇龙 | Method for preparing N-carbamyl glutamic acid |
| CN101481336A (en) * | 2009-01-19 | 2009-07-15 | 南昌大学 | Preparation of N-carbamoyl-aminoglutaric acid and sodium salt thereof |
| CN103980163A (en) * | 2014-05-30 | 2014-08-13 | 南京工业大学 | Method for continuously synthesizing N-carbamylglutamic acid by using microchannel reactor |
| CN105601542A (en) * | 2016-01-08 | 2016-05-25 | 南京工业大学 | Method for crystallizing N-carbamylglutamic acid by using mixed acid |
| CN108484448A (en) * | 2018-04-27 | 2018-09-04 | 湖北泓肽生物科技有限公司 | The method of one pot process N- carbamylglutamic acids |
Non-Patent Citations (1)
| Title |
|---|
| 刘雅倩: "N-氨甲酰谷氨酸合成及其生理功能研究", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
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