Method for preparing tetraethyl methylenediphosphonate

A technology of tetraethyl methylene diphosphate and diethyl chloromethylene phosphate is applied in the field of preparation of tetraethyl methylene diphosphate, and can solve the problems of being unsuitable for industrial production, complicated separation and difficult wastewater treatment. and other problems, to achieve the effect of easy industrialization, simple and safe process operation, and avoiding the difficulty of handling mixed solvents

Inactive Publication Date: 2016-10-12
肇庆巨元生化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the crude yield is as high as 90%, two aprotic solvents, THF and DMF, are used in large quantities in the reaction system, resulting in the final reaction system being a mixture of three solvents, and the separation is particularly complicated and difficult. In addition, part of THF and DMF are dissolved in the water phase, resulting in waste water It is also particularly difficult to handle and is not suitable for industrial production

Method used

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  • Method for preparing tetraethyl methylenediphosphonate
  • Method for preparing tetraethyl methylenediphosphonate
  • Method for preparing tetraethyl methylenediphosphonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The preparation method of tetraethyl methylene diphosphate comprises the following steps:

[0048] 1)

[0049] 1-1) Under nitrogen protection, add 4 moles (purity 99.03%) sodium ethoxide solid powder and 800mL absolute ethanol to a 2000mL single-port reaction flask equipped with a magnetic stirrer, stir and disperse, release the heat of dissolution, and take 20min, sodium ethoxide After dissolving and dispersing, part of the ethanol was distilled off under reduced pressure, and the ethanol was distilled off under reduced pressure to 50mbar at 60°C until sodium ethoxide solid was precipitated, which was beige, and 200mL of ethanol was recovered;

[0050] 1-2) Add 4 moles (purity: 99.93%) of diethyl phosphite to the sodium ethoxide solid obtained in 1-1), stir and dissolve for 5 minutes at 20°C to obtain a sodium diethyl phosphite ethanol solution;

[0051]1-3) Remove the ethanol in the ethanol solution of sodium diethyl phosphite obtained in 1-2) under reduced pressure ...

Embodiment 2

[0058] The preparation method of tetraethyl methylene diphosphate comprises the following steps:

[0059] 1)

[0060] 1-1) Under nitrogen protection, add 4.08 moles (purity 99.03%) sodium ethoxide solid powder and 750mL absolute ethanol to a 2000mL single-port reaction flask equipped with a magnetic stirrer, stir and disperse, release the heat of dissolution, and take 8min. After dissolving and dispersing, part of the ethanol was distilled off under reduced pressure, and the ethanol was distilled off under reduced pressure to 50mbar at 60°C until sodium ethoxide solid was precipitated, which was beige, and 120mL of ethanol was recovered;

[0061] 1-2) To the sodium ethoxide solid obtained in 1-1), add 4 moles (99.93% purity) of diethyl phosphite, stir and dissolve for 10 minutes at 50°C to obtain an ethanol solution of sodium diethyl phosphite;

[0062] 1-3) Remove the ethanol in the ethanol solution of sodium diethyl phosphite obtained in 1-2) under reduced pressure to 35 mb...

Embodiment 3

[0070] The preparation method of tetraethyl methylene diphosphate comprises the following steps:

[0071] 1)

[0072] 1-1) Under nitrogen protection, add 4.4 moles (purity 99.03%) sodium ethoxide solid powder and 1000mL absolute ethanol to a 2000mL single-port reaction flask equipped with a magnetic stirrer, stir and disperse, release the heat of dissolution, and take 30min, sodium ethoxide After dissolving and dispersing, part of the ethanol was distilled off under reduced pressure, and the ethanol was evaporated under reduced pressure to 50mbar at 60°C until sodium ethoxide solid was precipitated, which was beige, and 180mL of ethanol was recovered;

[0073] 1-2) Add 4 moles (purity: 99.93%) of diethyl phosphite to the sodium ethoxide solid obtained in 1-1), stir and dissolve for 30 minutes at 35°C to obtain an ethanol solution of sodium diethyl phosphite;

[0074] 1-3) Remove the ethanol in the ethanol solution of sodium diethyl phosphite obtained in 1-2) under reduced pre...

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Abstract

The invention discloses a preparation method of tetraethyl methylene diphosphate, comprising the following steps: 1) under the action of sodium ethoxide, diethyl phosphite reacts with sodium ethoxide to obtain sodium diethyl phosphite ethanol solution , ethanol is removed by distillation under reduced pressure to obtain sodium diethyl phosphite solid; 2) dichloromethane is added to the solid sodium diethyl phosphite obtained in step 1); sodium diethyl phosphite and dichloromethane are substituted After the reaction, tetraethyl methylene diphosphate was obtained. The preparation method of the invention has mild and simple reaction conditions and high yield at the same time. The method is simple to operate and low in energy consumption, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of tetraethyl methylene diphosphate. Background technique [0002] Tetraethyl methylene diphosphate is widely used as an important intermediate in the preparation of medicines, feed additives, food additives, etc. -1-cyclohexen-1-yl)-2,4-pentadienyl diethyl phosphate) fragments such as 3-methyl-5-(2,6,6-trimethyl -1-cyclohexen-1-yl)-1,3-pentadiene phosphate diethyl ester, 3-methyl-5-(2,6,6-trimethyl-1-cyclohexene-1- base)-2,4-pentadienyl phosphate diethyl ester, 3,7,11-trimethyl-1,3,6,10-carbapentadetracenyl phosphate diethyl ester, 3,7,11-tri The important intermediates of methyl-2,4,6,10-carbapentadetracenyl phosphate, etc., and these carbon 15 are important intermediates for the synthesis of vitamin A, β-carotene, apo-12'-carotene, An important intermediate of lycopene. Therefore, researching the synthetic method of tetraethyl me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40
CPCC07F9/4006
Inventor 廖艳金刘庆辉廖元统
Owner 肇庆巨元生化有限公司
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