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Preparation method for synthesizing vitamin A intermediate tetraethyl methylenediphosphonate

A technology of tetraethyl methylene diphosphonate and diethyl phosphite, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve problems that are not suitable for industrial production , Difficult waste water treatment, difficulty in mechanical application, etc., to achieve the effect of facilitating recycling, shortening reaction time, and facilitating follow-up reactions

Pending Publication Date: 2020-12-01
ZHEJIANG MEDICINE CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, THF and DMF exist in a large amount in the system, resulting in the mixing of the three solvents, which is difficult to separate and apply mechanically. In addition, part of THF and DMF is incorporated into the wastewater, which makes wastewater treatment difficult and is not suitable for industrial production.

Method used

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  • Preparation method for synthesizing vitamin A intermediate tetraethyl methylenediphosphonate
  • Preparation method for synthesizing vitamin A intermediate tetraethyl methylenediphosphonate
  • Preparation method for synthesizing vitamin A intermediate tetraethyl methylenediphosphonate

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1: the preparation of tetraethyl methylene diphosphate

[0031] (1) Under the condition of nitrogen protection, accurately weigh the solid sodium metal (23.69 g, 1.03 mol) and place it in a 500 ml four-neck flask.

[0032] (2) In step (1), put the four-necked flask in the sodium metal solid, add 100 ~ 150ml tetrahydrofuran, dropwise add diethyl phosphite (138.1g, 1.0mol) to control the reaction temperature at 15 ~ 25 ° C, drop After adding for 2 hours, after dropping, keep warm at 20-25°C for 10 hours to obtain a sodium diethyl phosphite solution, and precipitate to obtain a solid sodium diethyl phosphite.

[0033] (3) Dissolve the diethyl phosphite sodium salt in step (2) with 425g methylene chloride (5.0mol). React at a temperature of 25-30°C for 42-50 hours, add 200ml of water to terminate the reaction, and separate the liquids. The upper aqueous phase was extracted twice, the organic phases were combined, and distilled under reduced pressure to obtain t...

Embodiment 2

[0035] The operating steps are the same as in Example 1, except that the type of alkali in step (1) is changed, and sodium hydride is used as the alkali to prepare sodium diethyl phosphite, which is then reacted with dichloromethane to prepare tetramethylene diphosphonate ethyl ester. The fine GC content is 97.5%, and the yield is 80.5%.

Embodiment 3

[0037] The operation steps are the same as in Example 1, the difference is that the type of alkali in step (1) is changed, and sodium ethylate is used as alkali to prepare sodium diethyl phosphite, which is then reacted with dichloromethane to prepare tetramethylene diphosphonate ethyl ester. The fine GC content is 97.0%, and the yield is 76.6%.

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Abstract

The invention relates to a preparation method for synthesizing a vitamin A intermediate tetraethyl methylenediphosphonate. The preparation method comprises the following steps: adding an organic solvent into metallic sodium or a metallic sodium compound, uniformly stirring, dropwise adding diethyl phosphite at 10-60 DEG C, and keeping the temperature at 10-60 DEG C after the diethyl phosphite is dropwise added, so as to obtain a sodium diethyl phosphite solution; removing the organic solvent, and recovering the organic solvent to obtain a sodium diethyl phosphite solid; adding dichloromethaneinto the sodium diethyl phosphite salt for dissolving, and carrying out a substitution reaction at 20-55 DEG C, so as to obtain the tetraethyl methylenediphosphate. The method is simple and convenientto operate, short in process flow, less in involved solvent, simple and convenient to recycle, economic, environment-friendly, good in product quality and high in yield. Industrial production conditions can be met.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a specific synthesis method of tetraethyl methylene diphosphonate, an intermediate of vitamin A. Background technique [0002] Vitamin A (also known as retinol), has a variety of physiological functions, can maintain and promote human growth, development, reproduction and the stability of cell membranes, and has a significant effect on the formation of vision. It is one of the essential nutrients for the human body. Essential micronutrients for children's growth and development. Because of its anti-inflammatory, anti-oxidation, immune regulation, anti-skin aging, anti-cancer and other effects, it has been widely used in food, medicine, nutritional health products, cosmetics, feed additives, etc. Tetraethyl methylene diphosphate is an important intermediate in the synthesis of vitamin A and has great industrial value. [0003] The molecular structural formula of tetraethyl methyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
CPCC07F9/11
Inventor 黑延琳梁智平宋少奇贾建伟白亚龙王红卫
Owner ZHEJIANG MEDICINE CO LTD
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