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Preparation method of L-homoserine

A technology of homoserine and methionine, which is applied in the preparation of organic compounds, organic chemical methods, cyanide reaction preparation, etc., can solve the problems of high price of methyl iodide, unfavorable production amplification, complicated operation, etc., and reduce the use of toxic solvents. , Easy to operate, less dosage effect

Active Publication Date: 2019-09-27
CHENGDU BAISHIXING SCI & TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has the disadvantages of expensive methyl iodide as a raw material, high toxicity, low boiling point, a large amount of excess during use, a large amount of use, complicated reactions, and cumbersome operations, which are not conducive to further production scale-up.

Method used

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  • Preparation method of L-homoserine
  • Preparation method of L-homoserine

Examples

Experimental program
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Effect test

Embodiment 1

[0023] S1: In a 3-liter three-necked flask, add 1,500 grams of water, then 298 grams of L-methionine, stir well, then add 260 grams of concentrated hydrochloric acid, stir until clear, then add 441 grams of dimethyl sulfate dropwise at 25°C , stirred at room temperature for two days, spotted the plate to monitor the disappearance of the raw materials, and obtained the L-methionine sulfonium salt reaction liquid;

[0024] S2: The L-methionine sulfonium salt reaction solution obtained in S1 is heated to a reflux state for reaction, then slowly drips a saturated potassium bicarbonate solution (100 grams of potassium bicarbonate is dissolved in 500 grams of water), and the dropwise process controls the pH at 3- -6, continue to reflux reaction for 6 hours after dripping, and the raw materials basically disappear by pointing board monitoring;

[0025] S3: Lower the reaction solution to room temperature, then condense the film to remove most of the water, pre-cool the concentrate to ...

Embodiment 2

[0027] S1: In a 5-liter three-neck flask, add 2250 grams of water, then add 447 grams of L-methionine, stir well, then add 390 grams of concentrated hydrochloric acid, stir until clear, then add 661 grams of dimethyl sulfate dropwise at 25°C , stirred at room temperature for two days, spotted the plate to monitor the disappearance of the raw materials, and obtained the L-methionine sulfonium salt reaction solution.

[0028] S2: The above-mentioned L-methionine sulfonium salt reaction liquid is heated up to reflux state for reaction, and then slowly add saturated potassium bicarbonate solution (150 grams of potassium bicarbonate dissolved in 750 grams of water), and the pH is controlled at 3-- 6. Continue the reflux reaction for 6 hours after the dripping is completed, and the raw materials basically disappear by pointing the board monitoring.

[0029] S3: Lower the reaction solution to room temperature, then condense the film to remove most of the water, pre-cool the concentra...

Embodiment 3

[0031] S1: In a 2-liter three-neck flask, add 1000 grams of water, then 179 grams of L-methionine, stir well, then add 156 grams of concentrated hydrochloric acid, stir until clear, then add 265 grams of dimethyl sulfate dropwise at 25 °C , stirred at room temperature for two days, spotted the plate to monitor the disappearance of the raw materials, and obtained the L-methionine sulfonium salt reaction solution.

[0032] S2: The above-mentioned L-methionine sulfonium salt reaction solution is heated to reflux state for reaction, then slowly add saturated potassium bicarbonate solution (60 grams of potassium bicarbonate dissolved in 300 grams of water), and the pH is controlled at 3-- 6. Continue the reflux reaction for 6 hours after the dripping is completed, and the raw materials basically disappear by pointing the board monitoring.

[0033] S3: Lower the reaction solution to room temperature, then condense the film to remove most of the water, pre-cool the concentrated solut...

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Abstract

The invention belongs to the technical field of organic chemistry, and discloses a preparation method of L-homoserine, which comprises the following steps of S1, regulating L-methionine to be acidic with concentrated hydrochloric acid, then reacting with slightly excessive dimethyl sulfate at room temperature to produce an L-methionine sulfonium salt aqueous solution; S2, heating the L-methionine sulfonium salt aqueous solution obtained in the step S1 to reflux, then dropwise adding a saturated potassium bicarbonate solution, performing thermal cracking to remove dimethyl sulfide, so as to obtain a crude L-homoserine aqueous solution; S3, concentrating the crude L-homoserine aqueous solution obtained in the step S2, performing pre-cooling, removing salt with cation exchange resin, concentrating and crystallizing an eluent to obtain free crude L-homoserine, then adding acetone to perform pulping treatment on the crude L-homoserine to obtain high-purity L-homoserine. The method has the advantages that the raw materials are cheap and easy to obtain, the operation is simple, the cost is low, and is suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a preparation method of L-homoserine. Background technique [0002] L-homoserine and its derivatives are the structural precursors and synthetic building blocks of important physiologically active substances, which are widely used in the synthesis of various active substances, and are increasingly valued by scientific researchers. There are two main sources of L-homoserine: fermentation method and synthesis method. The current mainstream method is the synthesis method, which is to generate methyl sulfide by reacting L-methionine and methyl iodide, and then reflux under weak alkaline conditions to remove sulfide. After the reaction is completed, concentrate to remove salt, and use a solvent to react and crystallize to remove salt. However, this method has the disadvantages of expensive methyl iodide as a raw material, high toxicity, low boiling point, a larg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/16C07C229/22C07C227/40
CPCC07C227/16C07C381/12C07C227/40C07B2200/07C07C229/22
Inventor 石常青
Owner CHENGDU BAISHIXING SCI & TECH IND
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