Method for preparing N-acetyl-L-tyrosine

A technology of tyrosine and acetyl, applied in the field of preparing N-acetyl-L-tyrosine, which can solve the problems of high substance content, high production cost, and large energy consumption

Pending Publication Date: 2022-07-08
WUHAN GRAND HOYO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The current N-acetyl-L-tyrosine production process has defects such as high content of related substances, low yield, low optical

Method used

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  • Method for preparing N-acetyl-L-tyrosine
  • Method for preparing N-acetyl-L-tyrosine
  • Method for preparing N-acetyl-L-tyrosine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In this example, N-acetyl-L-tyrosine was prepared according to the following steps, and the process flow diagram is shown in figure 1 :

[0037] Step 1. Disperse 100 g of L-tyrosine in 200 ml of water, stir quickly to avoid agglomeration.

[0038] Step 2. Add 30% sodium hydroxide solution dropwise until the L-tyrosine is completely dissolved, pH=12.05.

[0039] 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.

[0040] 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.

[0041] Step 5. Add industrial hydrochloric acid to adjust the pH of the solution to 1.72.

[0042] 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.

[0043] Step 7, after bei

Embodiment 2

[0050] In this example, N-acetyl-L-tyrosine was prepared as follows:

[0051] Step 1. Disperse 500 grams of L-tyrosine in 1 liter of water and stir quickly to avoid agglomeration.

[0052] Step 2. Add 30% sodium hydroxide solution dropwise until the L-tyrosine is completely dissolved, pH=11.80.

[0053] Step 3. Add 296.3 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.

[0054] Step 4. After adding acetic anhydride, adjust pH=11.22 with sodium hydroxide solution, and keep the temperature at 60°C for 20 minutes.

[0055] Step 5. Add industrial hydrochloric acid to adjust the pH of the solution to 1.90.

[0056] Step 6, control the vacuum to be above 0.08MP, and concentrate under reduced pressure at 60-80°C until the reaction solution is basically in a solid state.

[0057] Step 7. After cooling to 4°C for full crystallization, the material is thrown away to obtai

Embodiment 3

[0063] In this example, N-acetyl-L-tyrosine was prepared as follows:

[0064] Step 1. Disperse 100 grams of L-tyrosine in 100 ml of water, stir quickly to avoid agglomeration.

[0065] Step 2. Put the high-quality mother liquor of Example 1 and the washed insoluble matter (L-tyrosine) into the reaction vessel together.

[0066] Step 3. Add 30% sodium hydroxide solution dropwise until L-tyrosine is completely dissolved, pH=12.25.

[0067] Step 4. Add 59.2 grams (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.

[0068] Step 5. After adding acetic anhydride, adjust pH=10.99 with sodium hydroxide solution, and keep the temperature at 60°C for 30 minutes.

[0069] Step 6, adding industrial hydrochloric acid to adjust the pH of the solution to 1.87.

[0070] Step 7, control the vacuum to be above 0.08MP, and concentrate under reduced pressure at 80°C until the reaction

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Abstract

The invention provides a method for preparing N-acetyl-L-tyrosine. The method comprises the following steps: carrying out acylation reaction on acetic anhydride and L-tyrosine under an alkaline condition to obtain acylation liquid; adjusting the pH value of the acylation solution to increase by using alkali liquor, carrying out heat preservation reaction, and then adjusting the pH value of the obtained reaction solution by using acid liquor to obtain a reaction solution containing N-acetyl-L-tyrosine; and carrying out purification treatment on the reaction liquid containing the N-acetyl-L-tyrosine. The N-acetyl-L-tyrosine prepared by the method has the advantages of high yield, low content of related substances, high optical purity and the like, and the method is low in energy consumption, low in production cost and suitable for large-scale production and application.

Description

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Claims

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Application Information

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Owner WUHAN GRAND HOYO
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