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A kind of synthetic method of trimethylphosphine oxide

A technology of trimethylphosphine oxide and synthesis method, which is applied in the field of synthesis of trimethylphosphine oxide, can solve the problems of difficult recovery and reuse of solvents, long reaction time, and low purity of products, and achieve easy recovery and reuse and initiation speed Fast and high product purity

Active Publication Date: 2017-12-19
SHANDONG WEITIAN FINE CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current method for preparing trimethylphosphine oxide has a long reaction time, the solvent is not easy to recycle and reuse, and the yield is low, and the product purity is low. In addition, the use of ether as a solvent is poor in safety

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of synthetic method of trimethylphosphine oxide, comprises steps:

[0022] 1) Preparation of Methylmagnesium Chloride

[0023] Under the protection of nitrogen, add 50 mL of mixed solvent and 1 mL of bromoethane into the reaction vessel containing 1 mol of magnesium chips. After heating to 50°C, slowly inject 15 g of methyl chloride into the reaction vessel. Continue to add 450 mL of mixed solvent; keep 45-50 ° C, continue to pass through 35 g of methyl chloride, after the completion, stir at 50 ° C for 2 hours to obtain methylmagnesium chloride; the mixed solvent is a mixed solvent of toluene and tetrahydrofuran, toluene The volume ratio with tetrahydrofuran is 2:1;

[0024] 2) Preparation of trimethylphosphine oxide

[0025] When the reaction solution obtained in step 1) is cooled to 5°C, add 2g of anhydrous copper chloride, then slowly drop in 51g of phosphorus oxychloride, stir for 2 hours after the drop (keep the temperature at 5°C during the dropping proc...

Embodiment 2

[0027] 1) Preparation of Methylmagnesium Chloride

[0028] Under the protection of nitrogen, add 50 mL of mixed solvent and 1 mL of bromoethane into the reaction vessel containing 1 mol of magnesium chips. After heating to 50°C, slowly inject 15 g of methyl chloride into the reaction vessel. Continue to add 450 mL of mixed solvent; keep 45-50 ° C, continue to pass through 35 g of methyl chloride, after the completion, stir at 50 ° C for 2 hours to obtain methylmagnesium chloride; the mixed solvent is a mixed solvent of toluene and tetrahydrofuran, toluene The volume ratio with tetrahydrofuran is 2:1;

[0029] 2) Preparation of trimethylphosphine oxide

[0030] When the reaction solution obtained in step 1) is cooled to 5°C, add 2g of anhydrous copper chloride, then slowly drop in 51g of phosphorus oxychloride, stir for 2 hours after the drop (keep the temperature at 5°C during the dropping process), and then add 200mL of water and 10mL of hydrochloric acid with a mass fracti...

Embodiment 3

[0032] A kind of synthetic method of trimethylphosphine oxide, comprises steps:

[0033] 1) Preparation of Methylmagnesium Chloride

[0034] Under the protection of nitrogen, add 50 mL of mixed solvent and 1 mL of bromoethane into the reaction vessel containing 1 mol of magnesium chips. After heating to 50°C, slowly inject 15 g of methyl chloride into the reaction vessel. Continue to add 450 mL of mixed solvent; keep 45-50 ° C, continue to pass through 35 g of methyl chloride, after the completion, stir at 50 ° C for 2 hours to obtain methylmagnesium chloride; the mixed solvent is a mixed solvent of toluene and tetrahydrofuran, toluene The volume ratio with tetrahydrofuran is 2:1;

[0035] 2) Preparation of trimethylphosphine oxide

[0036] When the reaction solution obtained in step 1) is cooled to 5°C, add 2g of anhydrous copper chloride, then slowly drop in 51g of phosphorus oxychloride, stir for 2 hours after the drop (keep the temperature at 5°C during the dropping proc...

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Abstract

The invention discloses a method for synthesizing trimethylphosphine oxide and belongs to the field of compound preparation. The method includes: under nitrogen protection, allowing chloromethane and magnesium chips to react in the mixed solution of toluene and tetrahydrofuran by using bromoethane as initiator so as to obtain methylmagnesium chloride; directly adding trichlorine into the methylmagnesium chloride, which needs not to be purified, after cooling, stirring under low temperature to allow for reaction, extracting after the reaction is completed, and performing vacuum refinery distillation and cooling crystallization to obtain the trimethylphosphine oxide. The method has the advantages that the purity of the obtained trimethylphosphine oxide is above 99.5%, the yield of the trimethylphosphine oxide reaches 95%, and the solvent used by the method is easy to recycle.

Description

technical field [0001] The invention relates to the field of compound synthesis, in particular to a synthesis method of trimethylphosphine oxide. Background technique [0002] Trimethylphosphine oxide is a very important intermediate compound, and its application is very extensive. The current method for preparing trimethylphosphine oxide has a long reaction time, the solvent is not easy to recycle and reuse, and the yield is low, and the product purity is low. In addition, the use of diethyl ether as a solvent has poor safety. Contents of the invention [0003] In order to make up for the deficiencies of the prior art, the invention provides a safe and reliable synthesis method of trimethylphosphine oxide. The method of the invention has low reaction temperature, short reaction time, easy solvent recovery and high yield. [0004] Technical scheme of the present invention is: [0005] A kind of synthetic method of trimethylphosphine oxide, comprises steps: [0006] 1) P...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/53
CPCC07F9/5304
Inventor 刘玉真刘玉强黄守超李章波刘乾刘阳升
Owner SHANDONG WEITIAN FINE CHEM TECH CO LTD
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