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Method for preparing N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide

A technology of dimethoxyphosphoryl and hydroxymethyl, which is applied in the field of flame retardants, can solve the problems of low reaction efficiency, high preparation cost, and long reaction time, and achieve high reaction efficiency, short reaction time, and low reaction temperature Effect

Active Publication Date: 2012-06-06
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

In the above-mentioned method, the analogous compound dimethyl (3-amino-3-acylpropyl) phosphonate of N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide is prepared as a catalyst using sodium alcohol compound The reaction time is long, the reaction efficiency is low, and the preparation cost is high

Method used

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  • Method for preparing N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide
  • Method for preparing N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide
  • Method for preparing N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide

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preparation example Construction

[0027] The invention discloses a preparation method of N-hydroxymethyl-3-(dimethoxyphosphoryl)propionamide, comprising:

[0028] Acrylamide, dimethyl phosphite, and a catalyst are reacted in a solvent to obtain dimethyl (3-amino-3-acylpropyl) phosphonate, and the catalyst is a non-acidic compound of an alkaline earth metal;

[0029] Reaction of the dimethyl(3-amino-3-acylpropyl)phosphonate with formaldehyde affords N-methylol-3-(dimethoxyphosphoryl)propanamide.

[0030] The acrylamide, dimethyl phosphite and catalyst react in a solvent to obtain dimethyl (3-amino-3-acylpropyl) phosphonate, and the reaction formula is as shown in formula I, and the dimethyl phosphite The molar ratio of fat and acrylamide is preferably 1~1.2:1, more preferably 1~1.1:1,

[0031]

[0032] The catalyst is a non-acidic compound of alkaline earth metal, preferably one or more of magnesium oxide, magnesium hydroxide, calcium oxide, calcium hydroxide, calcium hydride, strontium oxide, strontium hyd...

Embodiment 1

[0045] Add 5.517g of dimethyl phosphite (48.15mmol), 3.200g of acrylamide (45mmol), 0.180g of powdered magnesium oxide (4.5mmol), 10mL of methanol, 2mg of copper acetate, and a magnetic stirring bar into a 50mL three-necked flask. , a glass thermometer is installed in the three-necked bottle, and the bottle mouth is connected with a spherical condenser;

[0046] Pump out the air in the three-necked bottle once, fill it with ordinary nitrogen, then place the three-necked bottle in a preheated oil bath at 50 degrees Celsius, and magnetically stir the reaction system. The temperature of the system begins to rise in about 3 minutes, and the system boils when the internal temperature reaches 71 degrees Celsius. , then the temperature of the system began to decrease. After 20 minutes, the internal temperature of the system was 61 degrees Celsius. The reaction was stopped, and the reaction product was obtained. The reaction product was filtered, and the nuclear magnetic test was carri...

Embodiment 2

[0049] Add 22.294g of dimethyl phosphite (240.75mmol), 15.975g of acrylamide (225mmol), 0.900g of powdered magnesium oxide (22.5mmol), 50mL of methanol, 10mg of copper acetate, and a magnetic stirrer into a 250mL three-necked flask. , a glass thermometer is installed in the three-necked bottle, and the bottle mouth is connected with a spherical condenser;

[0050] Pump out the air in the three-necked bottle once, fill it with ordinary nitrogen, then place the three-necked bottle in a preheated oil bath at 50 degrees Celsius, and magnetically stir the reaction system. The temperature of the system begins to rise in about 3 minutes, and the system boils when the internal temperature reaches 71 degrees Celsius. , then the temperature of the system began to decrease. After 20 minutes, the internal temperature of the system was 61 degrees Celsius. The reaction was stopped, and the reaction product was obtained. The reaction product was filtered, and the nuclear magnetic test was car...

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Abstract

The embodiment of the invention discloses a method for preparing N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide, which comprises the following steps of: leading acrylamide, dimethyl phosphite and a catalyst to react in a solvent to obtain dimethyl (3-amino-3-acyl propyl) phosphonate, wherein the catalyst is a nonacid compound of alkaline earth metal; leading dimethyl (3-amino-3-acyl propyl)phosphonate to react with formaldehyde to obtain the N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide. In the invention, the nonacid compound of alkaline earth metal is used as the catalyst. Because the nonacid compound of alkaline earth metal is solid matter, the reactants including acrylamide and dimethyl phosphite can be in good contact with the solid catalyst. Meanwhile, the surface of the solid catalyst has high catalyst concentration to ensure that the catalyst is easy to initiate the reaction. Thus, the preparation method provided by the invention ensures short reaction time and high reaction efficiency.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a preparation method of N-methylol-3-(dimethoxyphosphoryl)propionamide. Background technique [0002] With the development of human society and economy, people pay more and more attention to the research of flame-retardant textiles. Many developed countries have clear legislation stipulating that pajamas, bedding, aviation decorative fabrics, camping tents and other textiles for the elderly and children must be used. Flame retardant textiles. [0003] At present, there are two main types of durable flame-retardant treatments for pure cotton fabrics commonly used in the market: the British Proban process and the Swiss Pyrovatex CP process. The Proban process uses tetrahydroxymethylphosphorus chloride (THPC) as a flame retardant, and the production process is complex. In addition to dipping, baking, washing and other steps, ammonia fumigation and oxidation treatment are a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40B01J23/02B01J21/10
Inventor 汪志勇张金堂汪苏靖查正根
Owner UNIV OF SCI & TECH OF CHINA
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