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Preparation method of L-selenomethionine

A technology of selenomethionine and dimethyl sulfate, which is applied in the field of preparation of L-selenomethionine, can solve the problems that are not conducive to labor protection and environmental protection, have foul-smelling selenium-methanol gas, and are not environmentally friendly, so as to achieve the benefit of labor Conservation and environmental protection, mild conditions, easy separation effect

Inactive Publication Date: 2020-01-03
河北凡博医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] (2) The amount of waste water during the preparation of dimethyl diselenyl ether is extremely large, which is not environmentally friendly;
[0008] (3) In the process of preparing sodium selenium methoxide from dimethyl diselenyl ether, it is very easy to produce foul-smelling and highly toxic selenium-methanol gas, which is extremely unfavorable for labor protection and environmental protection

Method used

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  • Preparation method of L-selenomethionine

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preparation example Construction

[0020] The invention provides a method for preparing L-selenomethionine. Compound 1 and compound 2 react to form compound 3. Compound 3 is reduced by sodium borohydride and then reacted with dimethyl sulfate to obtain the final product L-selenomethionine. . The synthetic route is .

[0021] The method of the present invention comprises two steps of step A and step B.

[0022] Step A, react compound 1 and compound 2 in a solvent, filter after reaction to obtain green solid compound 3, wherein the solvent is water, ethanol or methanol, the reaction temperature is 0-60°C (preferably 20-40°C), and the reaction The time is 3-10 hours (preferably 4-6 hours).

[0023] Compound 1 is , Compound 2 is , compound 3 is .

[0024] The molar ratio of compound 1 and compound 2 is 1:0.8-4, preferably 1:0.9-2.

[0025] This step specifically includes:

[0026] Preparation of compound 1: add sodium hydroxide to water at room temperature, add selenium particles after the sodium hydro...

Embodiment 1

[0029] Add sodium hydroxide (4.0 g, 0.1 mol) into water (30 ml) at room temperature, add selenium particles (7.9 g, 0.1 mol) after the sodium hydroxide is completely dissolved, and then add hydrazine hydrate (6.4 g, 0.1 mol) dropwise ), the dropwise addition was completed, and the temperature was slowly raised to 35°C for 3 hours, under nitrogen protection, compound 2 [(26.3g, 0.1mol) dissolved in 60ml of water] was added dropwise at this temperature, and reacted at 35°C for 3 hours after the dropwise addition was completed. After the reaction was completed, the temperature of the reaction system was lowered to 5° C., suction filtered, and dried to obtain 18.76 g of a green solid with a crude yield of 79.8% and an HPLC purity of 95%.

Embodiment 2

[0031] Add sodium hydroxide (4.0 g, 0.1 mol) into ethanol (30 ml) at room temperature, add selenium particles (7.9 g, 0.1 mol) after the sodium hydroxide is completely dissolved, and then add hydrazine hydrate (6.4 g, 0.1 mol) dropwise ), the dropwise addition was completed, and the temperature was slowly raised to 40°C for 3 hours, protected by nitrogen, and compound 2 [(23.7g, 0.09mol) dissolved in 60ml of ethanol] was added dropwise at this temperature, and reacted at 40°C for 4 hours after the dropwise addition was completed. After the reaction was completed, the temperature of the reaction system was lowered to 5° C., suction filtered, and dried to obtain 20.6 g of a green solid, with a crude product yield of 60.4% and an HPLC purity of 92%.

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Abstract

The invention discloses a preparation method of L-selenomethionine, and belongs to the field of additives. The preparation method comprises the following steps of A. reacting a compound 1 with a compound 2 in a solvent, and filtering after reaction to obtain a green solid compound 3; B. firstly, reacting the compound 3 with sodium borohydride in a protic solvent for 1-10 hours, dripping dimethyl sulfate after the reaction time is reached, continuing to react for 1-5 hours, quenching by using acetic acid, filtering and drying to obtain the L-selenomethionine. The preparation method disclosed bythe invention has the beneficial effects that: 1. the compound 1 has mild condition and high yield; 2. the reaction condition of the compound 3 is mild, virulent and malodorous selenium sodium methoxide cannot be generated, and the labor protection and the environmental protection are facilitated; 3. the compound 3 is simple to separate and only needs to be centrifugally subjected to spin filtration, and the obtained product has high purity; and 4. the raw materials and reagents are commercially available, and the intermediate does not need to be separated in the preparation process of the L-selenomethionine, so that the operation is simple.

Description

technical field [0001] The invention belongs to the field of additives, and in particular relates to a preparation method of L-selenomethionine. Background technique [0002] Selenium is an indispensable trace element that plays a very important role in the human body. Selenium cannot be synthesized in the human body, and it is an element that is easily excreted. Therefore, the human body must maintain a sufficient amount of selenium every day to maintain the normal metabolism of the body. amount of selenium. In the human body, the lack of trace element selenium will lead to the decline of human immunity. With the growth of age, the amount of selenium stored in the human body decreases in an aggregated series. At the same time, with the rapid economic development, changes in dietary structure and living habits, environmental pollution and other reasons have also led to more serious selenium deficiency in modern people (Contemporary Chemical Research, 2017, 11: 135-136). ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C391/00
CPCC07B2200/07C07C391/00
Inventor 刘育王天峰李明江刘子博李仕恒
Owner 河北凡博医药科技有限公司
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