Sodium 4-phenylbutyrate(link:https://www.bloomtechz.com/synthetic-chemical/api-researching-only/sodium-phenylbutyrate-powder-cas-1716-12-7.html), is an organic compound that exists in the form of colorless or white solid crystals. The chemical formula is C10H11NaO2, the corresponding molecular weight is 186.19 g/mol, and it usually has no obvious odor. It has good solubility in water. It can also be dissolved in some organic solvents, such as methanol, ethanol, chloroform, etc. Relatively stable at high temperature. However, it may decompose if exposed to heat for prolonged periods of time. The aqueous solution is alkaline and has a high pH. It is a flammable substance that can burn under an open flame to produce carbon dioxide, water and organic gases. It has been widely used in some cosmetics and beauty products. It has moisturizing, antioxidant and antibacterial properties and is used to improve skin's texture, delay skin aging and prevent skin problems like acne. It also has some other application fields, such as neuroprotection, anti-epilepsy, treatment of angiotensin-converting enzyme deficiency, etc. In addition, it is also used as a laboratory reagent and plays a role in biomedical research.
Sodium 4-phenylbutyrate (4-phenylsodium phenylbutyrate) is an organic compound that can be prepared by various synthetic methods. The following are several common synthetic methods:
1. In situ generation method:
This method generates 4-phenylsodium phenylbutyrate in situ through the reaction.
- Reaction steps: add benzoic acid and bromobutane into the reactor, and carry out condensation reaction in the presence of alkali to generate 4-phenylbutyrate. Then, 4-phenylbutyrate is reacted with sodium hydroxide to form 4-phenylsodium phenylbutyrate.
C7H6O2 + C4H9Br → 4-phenylbutyrate
4-phenylbutyrate + NaOH → C10H13NaO2
2. Reaction method:
- Reaction equation: C10H12O2 + NaOH → C10H13NaO2
Synthetic steps:
1. Prepare reactants: 4-phenylbutyric acid (4-phenylbutyric acid) and base (such as sodium hydroxide or sodium carbonate). Also prepare the appropriate solvent.
2. Preparation of reaction apparatus: Under dry conditions, equip a suitable reaction vessel, such as a round bottom flask. Make sure the reactor has an inert atmosphere.
3. Preparation of reaction mixture: 4-phenylbutyric acid and an appropriate amount of base are dissolved in an appropriate solvent to form a reaction mixture. Commonly used solvents include ethanol, methanol, and the like.
4. Heating reaction: heating the reaction mixture to an appropriate reaction temperature, usually in the range of 75-100°C. In this step, the reaction proceeds for about several hours.
5. Stirring reaction: keep stirring the reaction mixture under appropriate stirring conditions to promote the progress of the reaction.
6. End of reaction: After the reaction was completed, the reaction mixture was cooled to room temperature.
7. Acidification treatment: Acidify the reaction mixture by adding an acidic solution such as hydrochloric acid. This will cause the resulting sodium salt to precipitate out.
8. Crystal precipitation: Sodium 4-phenylbutyrate crystals are precipitated by cooling the reaction mixture, diluting or adding an appropriate solvent.
9. Filtration and washing: Wash and filter the resulting precipitate with an appropriate solvent. This will remove impurities.
10. Drying and purification: Dry the product to a constant weight by an appropriate drying method, and perform necessary purification steps, such as recrystallization, etc.
11. Verification and identification: Use appropriate analytical techniques, such as mass spectrometry, infrared spectroscopy, etc., to identify and verify the obtained product.
3. Ammonification method:
Reaction equation:
C10H12O2 + NH3 → C10H13NaO2 synthesis steps:
1. Prepare reactants: 4-phenylbutyric acid (4-phenylbutyric acid) and ammonia (NH3). Also prepare the appropriate solvent.
2. Preparation of reaction apparatus: Under dry conditions, equip a suitable reaction vessel, such as a round bottom flask. Make sure the reactor has an inert atmosphere.
3. Dissolving reactants: Add 4-phenylbutyric acid, appropriate amount of ammonia gas and appropriate solvent into the reaction vessel. Commonly used solvents can be methanol, ethanol, etc.
4. Heating reaction: Heating the reaction vessel to an appropriate reaction temperature, usually under moderate heating conditions. The reaction temperature can be adjusted according to experimental requirements, usually between 50-100°C.
5. Stirring reaction: keep stirring the reaction mixture under proper stirring conditions to promote the reaction.
6. The end of the reaction: Depending on the progress of the reaction, the reaction time usually takes several hours to tens of hours. When the reaction was complete, the heating was stopped.
7. Cooling: Cool the reaction mixture to room temperature.
8. Acidification treatment: Acidify the reaction mixture by adding an acidic solution such as hydrochloric acid. This will cause the precipitation of 4-phenylammonium phenylbutyrate.
9. Crystal precipitation: Sodium 4-phenylbutyrate crystals are precipitated by cooling the reaction mixture, diluting or adding an appropriate solvent.
10. Filtration and washing: Wash and filter the resulting precipitate with an appropriate solvent. This will remove impurities.
11. Drying and purification: Dry the product to a constant weight by an appropriate drying method, and perform necessary purification steps, such as recrystallization, etc.
12. Verification and identification: Use appropriate analytical techniques, such as mass spectrometry, infrared spectroscopy, etc., to identify and verify the obtained product.
4. Photocatalytic method:
- Reaction steps: react 4-phenylbutyric acid with a suitable photosensitive catalyst (such as a derivative of stilbene) under ultraviolet light to generate 4-phenylsodium phenylbutyrate.
- Reaction equation: C10H12O2 + photosensitive catalyst + light irradiation → C10H13NaO2
It should be noted that when carrying out the above synthesis method, the experimental operation needs to follow the safety regulations, and the reaction conditions, solvents and catalysts should be selected within the applicable range. At the same time, it is recommended to refer to relevant scientific literature and manuals for more detailed operating procedures and specific experimental conditions.