Production method of N-alkyl substituted phosphoric triamide

A technology of hydrocarbyl substitution and phosphoric triamide, which is applied in the fields of chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of restricting large-scale industrial production, reducing reaction yield and prolonging reaction Time and other issues, to achieve the effect of inhibiting side reactions, increasing reaction yield, and speeding up reaction speed

Active Publication Date: 2016-03-16
江西吉翔医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It mainly includes two side reactions, one is that the hydrocarbyl amine group will be replaced by amino group to generate triamino-substituted phosphoric triamide; the other is that the generated product N-hydrocarbyl substituted phosphoric triamide and dichloride to form a dimer , or even polymers, such as: Greatly reduces the yield of the reaction, causing difficulties for the subsequent separation
At the same time, because this reaction is realized by ammonia gas, ammonia gas first needs to enter through the diffusion of the outer surface, then diffuse through the liquid film, and then react with dichloride in the solvent, so the solubility of ammonia gas in the solvent becomes a constraint A factor of the reaction, on the other hand, ammonia diffuses from the gas phase to the gas-liquid interface in the reaction process, a

Method used

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  • Production method of N-alkyl substituted phosphoric triamide
  • Production method of N-alkyl substituted phosphoric triamide

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0045] Example 1 (N-n-butyl thiophosphoric triamide)

[0046] Dissolve 25.43g of trichlorothion in 180g of ethyl acetate, put it into a four-necked flask equipped with stirring, add 15.18g of triethylamine first, and add 11.54g of n-butylamine dropwise to the ethyl acetate of trichlorothion Ester solution, the dropping time is kept at 1 hour, the holding time is 0.5 hour, the reaction temperature is controlled at -30 ℃, the content of phosphorus trichloride cannot be detected by sampling and analysis, and the reaction is terminated to obtain the reaction solution of the first step;

[0047] Open the ammonia gas cylinder and pass in ammonia gas. The ammonia gas passes through a cold hydrazine. From the outside, it can be seen that liquid ammonia gradually appears. Maintain the temperature at -45°C, add 12.75g of liquid ammonia, gradually add dropwise the reaction solution of the first step of precooling, start the reaction, and keep the dropping time at 1.5 hours. When the thi...

Example Embodiment

[0048] Embodiment 2 (N-n-propyl thiophosphoric triamide)

[0049] Dissolve 25.43g of thionyl chloride in 180g of ethyl acetate, put it into a four-necked flask equipped with stirring, add 15.18g of triethylamine first, and add 8.9g of n-propylamine dropwise to the ethyl acetate of thionyl chloride solution, the dropping time was kept at 1 hour, the holding time was 0.5 hour, the reaction temperature was controlled at -15°C, the content of phosphorus trichloride could not be detected by sampling and analysis, and the reaction was terminated to obtain the reaction solution of the first step;

[0050] Put the autoclave into the low temperature oil bath, keep the temperature in the autoclave at -20℃, close the lid of the autoclave, connect the ammonia gas cylinder to the autoclave, and pass the ammonia gas into the autoclave, at this time keep the pressure of the autoclave 0.18MPa, the temperature of the autoclave is kept at -20°C, and it can be observed that ammonia has become li...

Example Embodiment

[0051] Example 3 (mixture of N-n-butyl thiophosphoric triamide and N-n-propyl thiophosphoric triamide)

[0052] Dissolve 25.43g of phosphorous trichloride in 160g of ethyl acetate, put it into a four-necked flask equipped with stirring, first add 15.18g of triethylamine, and dropwise add 6.8g of n-butylamine and 3.54g of n-propylamine to sulfur trichloride Phosphorus in ethyl acetate solution, the dropping time was kept at 2h, the holding time was 1h, the reaction temperature was controlled at -10°C, the content of phosphorus trichloride could not be detected by sampling and analysis, the reaction was terminated, and the reaction solution of the first step was obtained;

[0053] Add 13g of liquefied ammonia into the reactor, keep the temperature in the reactor at -40°C, and dropwise add the reaction solution of the first step of precooling, the dropwise addition time is 1 hour, continue to maintain the temperature at -40°C for reaction, and take a sample to detect , when the u...

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Abstract

The invention relates to a production method of N-alkyl substituted phosphoric triamide. In an organic solvent, liquid ammonia reacts with alkyl amino phosphorodichloridate. The production method further comprises steps as follows: (1), phosphoric trichloride and alkyl primary amine react in the presence of the organic solvent and an acid-binding agent, and alkyl amino phosphorodichloridate is generated; (2), a reaction liquid in the step (1) directly reacts with the liquid ammonia, temperature returning is performed, and N-alkyl substituted phosphoric triamide is generated. The liquid ammonia is preferably added in the step (2), and a reaction liquid in the step (1) is added for a reaction. According to the production method, a procedure can be intermittent or continuous, an intermediate is not required to be purified, the reaction condition is mild, few byproducts are produced, the yield is good, the purity is high, and the production method is suitable for industrial production.

Description

field of invention [0001] The invention relates to a production method of urease inhibitor N-hydrocarbyl substituted phosphoric triamide, in particular to an industrialized production method of N-hydrocarbyl substituted phosphoric triamide. Background technique [0002] N-hydrocarbyl substituted phosphoric triamides are highly effective urokinase inhibitors. At present, urea, which is the most widely used in the world, must be converted into ammonium carbamate through the enzymatic hydrolysis of urokinase in the soil, and absorbed by plants in the form of ammonium nitrogen. Due to the high activity of urokinase in the soil, the conversion of urea to release amine nitrogen is very fast. Before the crops can absorb it, they will be lost as ammonia nitrogen volatilization. Part of the ammonium nitrogen absorbed by crops can also be converted into nitrate nitrogen, which will cause the deterioration of the atmosphere and soil environment through leaching and volatilization. N-...

Claims

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Application Information

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IPC IPC(8): C07F9/22
Inventor 王农跃瞿雄伟李国华茅晓晖
Owner 江西吉翔医药化工有限公司
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