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Synthesis and purification method of methyl phosphinate compounds

A technology of methyl phosphonite and dialkyl methyl phosphonite, which is applied in the field of synthesis and purification of methyl phosphonite compounds, can solve problems such as unrealistic industrialization, and achieve the reduction of methyl phosphonite The formation, excellent reaction yield and product quality, the effect of mild process conditions

Active Publication Date: 2015-12-09
HEBEI VEYONG BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From equipment to energy consumption to the decomposition of products, industrialization is unrealistic

Method used

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  • Synthesis and purification method of methyl phosphinate compounds
  • Synthesis and purification method of methyl phosphinate compounds
  • Synthesis and purification method of methyl phosphinate compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The synthesis of embodiment 1 diethyl methylphosphonite

[0062] Under the protection of nitrogen, add 15.6g (0.1mol) of diethyl phosphonite chloride and 30mL tetrahydrofuran into a four-necked flask, start stirring and cool down to -10°C, add dropwise a tetrahydrofuran solution of methylmagnesium chloride (20%, 41.1 g, 0.11mol), keep the temperature at -10~-5°C, control the gas phase, diethyl phosphonite chloride ≤0.5%.

[0063] Control the temperature at -20~-15°C, add 40mL of 20% sodium chloride solution and 0.5g of hexadecyltributylphosphorus chloride to the above reaction solution, solids are precipitated, filter, and distill the filtrate under reduced pressure to collect 60~ 70°C / 50mmHg fraction, 10.15g of diethyl methylphosphonite was obtained, content (GC) 95%, 1 HNMR (500Hz, CDCl 3 ) δ 1.37(3H,t, J =7.0Hz), 1.55(3H, d, J =15.0Hz),4.15(2H, J =7.0, J =63.7Hz),7.23(1H,d, J =539Hz).

Embodiment 2

[0064] The synthesis of embodiment 2 ethyl methylphosphonite

[0065] Under the protection of nitrogen, add 15.6g (0.1mol) of diethyl phosphonite chloride and 30mL tetrahydrofuran into a four-necked flask, start stirring and cool down to -10°C, add dropwise a tetrahydrofuran solution of methylmagnesium chloride (22%, 37.4g , 0.11mol), keep the temperature at -10~-5°C, control the gas phase, diethyl phosphonite chloride ≤0.5%.

[0066] Control the temperature at -5~0°C, add 50mL of 15% sodium chloride solution and 0.3g of cetyltributylammonium chloride to the above reaction solution, solid precipitates, filter, distill the filtrate under reduced pressure, collect 55~60 °C / 90mmHg fraction, 8.8 g of ethyl methylphosphite was obtained, with a content (GC) of 96%.

Embodiment 3

[0067] The synthesis of embodiment 3 dibutyl methylphosphonite

[0068] Under the protection of nitrogen, add 21.2g (0.1mol) of dibutyl phosphonite chloride and 40mL tetrahydrofuran into a four-necked flask, start stirring and cool down to -15°C, add dropwise a tetrahydrofuran solution of methylmagnesium chloride (21%, 39.1 g, 0.11mol), keep the temperature at -10~-5°C, control the gas phase, dibutyl chloride phosphonite ≤0.5%.

[0069] Control the temperature at -15~-20°C, add 50mL of 25% magnesium chloride solution and 0.2g of hexadecyltributylammonium bromide to the above reaction solution, solid precipitates, filter, distill the filtrate under reduced pressure, collect at 70~80°C / 50mmHg fraction to obtain 12.75g of dibutyl methylphosphonite, content (GC) 96%, 1 HNMR (500Hz, CDCl 3 ) δ 0.95(3H,t, J =7.5Hz), 1.38(2H,m), 1.55(3H,d, J =15.5Hz), 1.70(2H,m), 4.05(2H, J =7.0, J =63.5Hz),7.22(1H,d, J =538Hz).

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Abstract

The invention relates to a synthesis and purification method of methyl phosphinate compounds. The method concretely comprises the following steps: adding brine to a solution containing a methyldialkyl phosphinate and magnesium chloride mixture in an inert solvent at a low temperature, and separating to obtain methylalkyl phosphinate or methyldialkyl phosphinate. The method solves the post-treatment and purification difficulties of a Grignard reagent method, and has the advantages of industrial production, effective reduction of the generation of methyl phosphonous acid, mild process conditions, and excellent reaction yield and product quality.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a method for synthesizing and purifying methylphosphonite compounds. technical field [0002] The invention relates to the field of medicine and chemical industry, in particular to a method for synthesizing and purifying methylphosphonite compounds. Background technique [0003] Agricultural herbicides have brought many advantages to agricultural production, reduced the labor intensity of farmers, effectively controlled the growth of weeds in farmland, and improved the yield and quality of crops. As the world's largest total herbicide, glyphosate started early in its development. At present, it has entered a mature stage in terms of scale and technology, and the market is already saturated. Due to the continuous use for many years, the problem of weed resistance will inevitably occur, which will bring a series of problems such as control effect, drug cost, and phy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40C07F9/48
Inventor 王双珠马彩霞赵立峰刘洁史秀肖范立攀贾成国
Owner HEBEI VEYONG BIO CHEM
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