Tris Base, with a molecular formula of C3H8NO3, CAS 77-86-1, and a molecular weight of 121.1. Also known as Tris (hydroxide) aminomethane. White crystalline particles. Trihydroxymethylaminomethane is widely used in the treatment of acute metabolic and respiratory acidemia. It belongs to alkaline buffering agent and has a good buffering effect on metabolic acidosis and enzyme activity. The synthesis method of trihydroxymethylnitromethane is n (nitromethane): n (formaldehyde)=1:3.2, using Ca (OH) 2 solution as catalyst, adjusting the pH value to around 9, controlling the reaction temperature at 30 ℃, and reacting for 4 hours. At an hour, trihydroxymethylnitromethane was obtained with a yield of 91.3%. In ethanol and dichloromethane solvents, hydrazine hydrate is used as a reducing agent and a catalyst is added to reduce nitro groups. Apply the reduction method of aromatic nitro compounds to polyhydroxyaliphatic nitro compounds.
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Tris Base has multiple synthesis methods, and the following are three common synthesis methods:
Method 1:
Mix chloroform (CHCl3) and ammonia (NH3) in a certain molar ratio to produce tris (2-chloroethoxy) methylamine (Tris base) through the reaction. Then, by conducting an ammonolysis reaction on the Tris base, a Tris chelating agent is obtained.
1. Trichloromethane reacts with ammonia to form Tris base
Synthesis steps:
(1) Add an appropriate amount of trichloromethane and ammonia (in a molar ratio of 1:3) to a round bottom flask and stir with a magnetic stirrer.
(2) Stir the reaction mixture at room temperature for a certain period of time until the reaction is complete.
(3) Separate the upper clear liquid from the reaction solution through a separating funnel to obtain the crude product of Tris base.
(4) Recrystallize the crude Tris base, filter and dry to obtain the pure Tris base.
Chemical reaction equation:
CHCl3+3NH3 → N (CH2CH2Cl) 3+3H2O
2. Performing ammonolysis reaction on Tris base to obtain Tris chelating agent
Synthesis steps:
(1) Add an appropriate amount of Tris base and ammonia (in a molar ratio of 1:3) to a round bottom flask and stir with a magnetic stirrer.
(2) Stir the reaction mixture at room temperature for a certain period of time until the reaction is complete.
(3) Separate the upper clear liquid from the reaction solution through a separating funnel to obtain the crude Tris chelating agent.
(4) Recrystallize the crude Tris chelating agent, filter and dry to obtain the pure Tris chelating agent.
Chemical reaction equation:
N (CH2CH2Cl) 3+3NH3 → N (CH2CH2NH2) 3+3HCl
Through the above steps, we successfully generated Tris base through the reaction of trichloromethane and ammonia, and then obtained Tris chelating agent through ammonolysis of Tris base.
Method 2:
Tris base is generated by reacting formaldehyde with ammonium chloride or ammonium carbonate. Mix an appropriate amount of formaldehyde solution with ammonium carbonate or ammonium chloride aqueous solution, and stir at room temperature for 24 hours to obtain Tris alkaline solution. Then add hydrochloric acid dropwise to the Tris alkaline solution until the target pH value is reached. The final solution obtained is Tris buffer, which can be filtered and sterilized as needed.
Synthesis steps
1. Add an appropriate amount of formaldehyde aqueous solution and ammonium carbonate or ammonium chloride aqueous solution (molar ratio 1:3) to a round bottom flask, and stir with a magnetic stirrer.
2. Stir the reaction mixture at room temperature for a certain period of time (usually 24 hours) until the reaction is complete. During this process, the reaction will generate Tris bases and other byproducts.
3. Separate the upper clear liquid through a separating funnel to obtain Tris alkaline solution. In this step, appropriate organic solvents can be used for extraction to further purify Tris base.
4. In the collected Tris alkaline solution, use an appropriate amount of hydrochloric acid hydrochloric acid hydrochloric acid hydrochloric acid hydrochloric acid, add dropwise to the Tris alkaline solution until the target pH value is reached. During this process, it is necessary to closely monitor the pH value to avoid it being too low or too high.
5. Finally, Tris buffer can be filtered and sterilized as needed. For example, filters can be used to remove impurities from the solution, or appropriate sterilization methods can be used to ensure the sterility of the solution.
Chemical equation:
The reaction between formaldehyde and ammonium carbonate or ammonium chloride can be expressed as:
HCHO+3NH4OH → N (CH2OH) 3+3H2O+HCO3-
Among them, HCHO is the chemical formula of formaldehyde, and NH4OH is an aqueous solution of ammonium carbonate or ammonium chloride. This reaction generates Tris base (N (CH2OH) 3) and bicarbonate ion (HCO3-).
The reaction of adding hydrochloric acid to adjust pH can be expressed as:
HCHO+3NH4OH → N (CH2OH) 3+3H2O+HCO3-
HCO3-+H+→ H2CO3 → CO2 ↑+H2O
In this reaction, the bicarbonate ion (HCO3-) combines with the hydrogen ion (H+) to form carbon dioxide and water (CO2 ↑+H2O). During this process, attention should be paid to controlling the reaction temperature and stirring speed to avoid the occurrence of side reactions. At the same time, hydrochloric acid needs to be added dropwise to avoid low or high pH values. In the steps of filtration and sterilization, appropriate filters can be used to remove impurities and insoluble substances from the solution. At the same time, appropriate sterilization methods can be used to ensure the sterility of the solution to meet the requirements of subsequent experiments.
Method 3:
Generate Tris base by reacting 1,3-propanediol with ammonium chloride or carbonate. Mix an appropriate amount of 1,3-propanediol with ammonium carbonate or ammonium chloride aqueous solution, and stir under heating conditions for a certain period of time to obtain Tris alkaline solution. Then add hydrochloric acid dropwise to the Tris alkaline solution until the target pH value is reached. The final solution obtained is Tris buffer, which can be filtered and sterilized as needed.
Synthesis steps:
1. Add an appropriate amount of 1,3-propanediol solution and ammonium carbonate or ammonium chloride aqueous solution (molar ratio 1:3) to a round bottom flask, and stir with a magnetic stirrer.
2. Stir the reaction mixture under heating conditions for a certain period of time (usually 24 hours) until the reaction is complete. During this process, the reaction will generate Tris bases and other byproducts. The purpose of heating is to promote the reaction and increase the yield of Tris base.
3. Separate the upper clear liquid through a separating funnel to obtain Tris alkaline solution. In this step, appropriate organic solvents can be used for extraction to further purify Tris base.
4. In the collected Tris alkaline solution, use an appropriate amount of hydrochloric acid hydrochloric acid hydrochloric acid hydrochloric acid hydrochloric acid, add dropwise to the Tris alkaline solution until the target pH value is reached. During this process, it is necessary to closely monitor the pH value to avoid it being too low or too high.
5. Finally, Tris buffer can be filtered and sterilized as needed. For example, filters can be used to remove impurities from the solution, or appropriate sterilization methods can be used to ensure the sterility of the solution.
Chemical synthesis reaction formula:
The reaction between 1,3-propanediol and ammonium carbonate or ammonium chloride can be expressed as:
HOCH2CH (OH) CH2OH+3NH4OH → N (CH2OH) 3+3H2O+CO32- or Cl-
Among them, HOCH2CH (OH) CH2OH is the structural formula of 1,3-propanediol, and NH4OH is an aqueous solution of ammonium carbonate or ammonium chloride. This reaction generates Tris base (N (CH2OH) 3) and carbonate ions (CO32-) or chloride ions (Cl -).
The reaction of adding hydrochloric acid to adjust pH can be expressed as:
CO32-+H+→ HCO3- → H2CO3- → CO2 ↑+H2O
Cl -+H+→ HCl → (g)+Cl - (aq)
Among them, HCO3- represents bicarbonate ions, H2CO3 represents carbonic acid, CO2 ↑ represents carbon dioxide gas, and H2O represents water. In these reactions, carbonate ions (CO32-) or chloride ions (Cl -) combine with hydrogen ions (H+) to form carbon dioxide gas and water, or hydrogen chloride gas and chloride ions (Cl -). During this process, attention should be paid to controlling the reaction temperature and stirring speed to avoid the occurrence of side reactions. At the same time, hydrochloric acid needs to be added dropwise to avoid low or high pH values.
These methods each have their own advantages and disadvantages, and need to be selected based on specific experimental conditions and requirements. In practical operation, it is also necessary to pay attention to safety issues and take corresponding protective measures.