N-Acetyl-L-tyrosine synthesis
- Product Name:N-Acetyl-L-tyrosine
- CAS Number:537-55-3
- Molecular formula:C11H13NO4
- Molecular Weight:223.23
Yield:6393-42-6 99.95%
Reaction Conditions:
with sodium hydroxide in lithium hydroxide monohydrate at 60; pH=8 - 12.05; for 0.333333 h;pH-value;
Steps:
1-3; 1-6
Step 1. Disperse 100 g of L-tyrosine in 200 ml of water, stir quickly to avoid agglomeration.Step 2. Add 30% sodium hydroxide solution dropwise until the L-tyrosine is completely dissolved, pH=12.05.Step 3. Add 59.2 g (1.05 times the molar amount) of acetic anhydride dropwise for 30 minutes, while adding 30% sodium hydroxide solution dropwise to maintain the pH between 8 and 10.Step 4. After adding acetic anhydride, dropwise add sodium hydroxide solution to adjust pH=11.50, and keep the temperature at 60°C for 20 minutes.Step 5. Add industrial hydrochloric acid to adjust the pH of the solution to 1.72.Step 6, control the vacuum to be above 0.08MP, and concentrate under reduced pressure at 80°C until the reaction solution is basically in a solid state.Step 7, after being cooled to 4 and fully crystallized, the material is dumped to obtain N-acetyl-L-tyrosine crude product I (containing the mixture of acetyl tyrosine, tyrosine, inorganic salt, a small amount of acid/water), mother liquor obsolete.Step 8. The obtained crude N-acetyl-L-tyrosine I was slurried with 3 times the volume of ethanol (95%) at 60° C. to extract N-acetyl-L-tyrosine.In step 9, the ethanol solution obtained in step 8 is concentrated under reduced pressure to recover the solvent, and crystallized to obtain crude N-acetyl-L-tyrosine II. The ethanol can be reused after recovery.Step 10. Add N-acetyl-L-tyrosine crude product II and an equal amount of purified water to the decolorization vessel. Stir and heat to 65 to dissolve, add 0.5% of the solid content of N-acetyl-L-tyrosine crude product II to decolorize for 10 minutes, decolorize and filter, the filtrate is cooled for crystallization, the filtrate is cooled to 4 and stirred until the crystals are completely precipitated, filtered , 100.05 grams of N-acetyl-L-tyrosine fine products were obtained after drying. During continuous production, the crystallization mother liquor of the refining process can be applied to step 1.After the extraction in step 11 and step 8, the obtained filter residue is dissolved in water to remove inorganic salts and some impurities, and the remaining insoluble matter is L-tyrosine, which can be applied back to step 1 in continuous production.
References:
CN114716335,2022,A Location in patent:Paragraph 0076-0137
1576-48-3
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