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Method for preparing novel metabolic accelerator butafosfan

A technology of butafosin and hypophosphorous acid, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. , Easy industrial production, high stability effect

Active Publication Date: 2012-12-05
青岛动保国家工程技术研究中心有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Butafosfos prepared by the prior art is very expensive, so it is of great significance to study a synthetic method of butafosfos with low cost and high yield

Method used

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  • Method for preparing novel metabolic accelerator butafosfan
  • Method for preparing novel metabolic accelerator butafosfan
  • Method for preparing novel metabolic accelerator butafosfan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 108kg of n-butylamine into the reaction kettle, add 300l of acetone, and dissolve 144kg of 98% hypophosphite in 50l of acetone, then add the acetone solution of hypophosphite into the solution of n-butylamine, stir for 3 hours, the system will The amine salt of hypophosphorous acid is precipitated. After the system was heated to reflux in a water bath for 4 hours, the reaction was terminated. Put the system in a cooling tank and leave it overnight, the product precipitates, filters, and centrifuges to obtain a crude product, then recrystallizes with a mixed system of 4 times the amount of methanol and acetone, keeps it warm for 1 hour, cools in a crystallization kettle, centrifuges, and dries to obtain 225kg of the product .

Embodiment 2

[0027] Put 108kg of n-butylamine into the reaction kettle, add 300l of acetone, and dissolve 155kg of 98% hypophosphite in 50l of acetone, then add the acetone solution of hypophosphite into the solution of n-butylamine, stir for 3 hours, the system will The amine salt of hypophosphorous acid is precipitated. After the system was heated to reflux in a water bath for 4 hours, the reaction was terminated. Put the system in a cooling tank and leave it overnight, the product precipitates, filters, and centrifuges to obtain a crude product, then recrystallizes with a mixed system of 4 times the amount of methanol and acetone, heats it for 1 hour, cools in a crystallization kettle, centrifuges, and dries to obtain 230kg of the product .

Embodiment 3

[0029] Put 108kg of n-butylamine into the reaction kettle, add 300l of acetone, and dissolve 165kg of 98% hypophosphite in 50l of acetone, then add the acetone solution of hypophosphite into the solution of n-butylamine, stir for 3 hours, the system will The amine salt of hypophosphorous acid is precipitated. After the system was heated to reflux in a water bath for 4 hours, the reaction was terminated. Put the system in a cooling tank and leave it overnight, the product precipitates, filters, and centrifuges to obtain a crude product, then recrystallizes with a mixed system of 4 times the amount of methanol and acetone, keeps it warm for 1 hour, cools in a crystallization kettle, centrifuges, and dries to obtain 235kg of the product .

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Abstract

The invention relates to the technical field of preparation of veterinary medicine and provides a method for preparing novel metabolic accelerator butafosfan. The method includes using n-butylamine, acetone, hypophosphorous acid as raw materials, condensating the n-butylamine and the acetone to generate imine, and reducing by hypophosphorous acid. Specifically, the method includes the steps of adding the n-butylamine and the aceton into a reactor, stirring at room temperature, dropping hypophosphorous acid into the acetone solution, controlling the reaction temperature within 40 DEG C; cooling and filtering after backflow reaction, and centrifuging to obtain crude products; adding the crude products into a crystallizing reactor, adding the acetone / methyl alcohol solution, heating to backflow, cooling, centrifuging and drying to obtain finish products. The method for preparing novel metabolic accelerator butafosfan is low in material cost, short in steps, high in operability, low in pollution and high in yield, and the total yield of target compounds is 90% around.

Description

technical field [0001] The invention belongs to the technical field of preparation of veterinary drugs, and mainly relates to a preparation method of a metabolism accelerator butafosfos. Background technique [0002] Butafosfos was developed by German Bayer Company for many years and approved the aminoprofos compound of listing in 1958. The chemical name is 1-(butylamino)-1-methylethyl]-phosphonic acid, and the English name is Butafosfan; (1 -Butylamino-1-methyl-ethyl)-phosphinic acid; Molecular formula is C 7 h 18 NO 2 P; molecular weight: 179.20 [0003] The structural formula is: [0004] [0005] The purpose of developing this compound at that time was to solve the comprehensive disorders such as calcium and magnesium metabolism disorders, decreased body immunity, and body dysfunction caused by nutritional imbalances and various stress responses in large animals. After 20 years of market application, not only the compound and vitamin B 12 The mixed preparation c...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 郝智慧姚德勇贾德强林扬沈巍王艳玲
Owner 青岛动保国家工程技术研究中心有限公司
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