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Amino arene structure unit-containing polyacrylate functionalized polymer and preparation method thereof

A technology of structural units and aminoaromatics, applied in the direction of organic chemistry, can solve the problems of high yield, low product cost, high price, etc., and achieve the effect of high yield, less waste water, and simple preparation method

Active Publication Date: 2013-07-10
XINFA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the present three kinds of routes about the synthesis of 2-methyl-4-amino-5-aminomethylpyrimidine all have various drawbacks: such as the cyanopyrimidine route needs to use a large amount of ethyl acetimide hydrochloride (1.8 to 2 equivalents), the raw material and malononitrile are expensive, which is not conducive to the reduction of product cost; the reaction steps of the formyl pyrimidine route are complicated, the reaction cycle is long, and an autoclave (about 50 kg pressure) is used for hydrogenation reaction, which is difficult to implement industrially ; and the formylaminopyrimidine route takes 3-aminopropionitrile as starting raw material, although the raw material of this route is cheap and easy to get, the reaction conditions of each step are relatively mild, and the yield is higher, which is conducive to product cost control
But this route has fatal disadvantages: it uses highly carcinogenic o-chloroaniline, which requires high operating environment and is not conducive to environmental protection; and despite steam distillation and multiple recrystallizations, it is still difficult to remove trace amounts of o-chloroaniline in the final product vitamin B1. Chloroaniline

Method used

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  • Amino arene structure unit-containing polyacrylate functionalized polymer and preparation method thereof
  • Amino arene structure unit-containing polyacrylate functionalized polymer and preparation method thereof
  • Amino arene structure unit-containing polyacrylate functionalized polymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Add 400 grams of isopropanol, 100 grams of deionized water, and 95.5 grams (0.5 moles) of 2-(2-aminobenzene) ethanol acrylate into a 1000 ml stainless steel reactor; heat to an internal temperature of 65-75 degrees, drop 1.6 A solution of 1 gram of octyl peroxide and 10 grams of isopropanol, after dropping, the temperature was raised to 85-95°C, and the reaction was carried out for 5 hours. Alkyl mercaptan, heat preservation reaction for 2 hours; filter while hot, remove a small amount of high molecular weight polymer; filtrate is cooled to room temperature, filter, dry, obtain (formula 1) poly 2-(2-aminophenyl) ethanol acrylate 77.4 grams , the appearance is off-white solid particles, the number average molecular weight ranges from 4000 to 12000, swells in hot water, soluble in hot alcohol, and the yield is 81.0%.

Embodiment 2

[0041] Use 95.5 grams of 2-(3-aminophenyl)ethanol acrylate as a monomer to replace 2-(2-aminophenyl)ethanol acrylate in Example 1 for free radical polymerization. The specific process of the reaction is the same as in Example 1. The material yield is shown in Table 1.

Embodiment 3

[0043] Use 95.5 grams of 2-(4-aminophenyl)ethanol acrylate as a monomer to replace 2-(2-aminophenyl)ethanol acrylate in Example 1 for free radical polymerization. The specific process of the reaction is the same as in Example 1. The material yield is shown in Table 1.

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Abstract

The invention relates to an amino arene structure unit-containing polyacrylate functionalized polymer and a preparation method thereof. The preparation method comprises the steps of: by utilizing a method of initiating solution polymerization through free radicals, initiating an amino arene structure unit-containing polyacrylate monomer to be in free radical polymerization in an alcohol-water solvent, performing molecular weight regulation to the polymer by lauryl mercaptan, separating according to different solubilities of polymers with different molecular weights in the alcohol-water system to obtain the amino arene structure unit-containing polyacrylate functionalized polymer with the molecular weight range of 4,000-12,000. The functionalized polymer can be used for entirely replacing o-chloroaniline for preparing vitamin B1, can be recycled after being filtered, the preparation method is simple and convenient to operate, and high in yield, thereby being an industrialized green and environment-friendly production method with the raw material cost advantage.

Description

technical field [0001] The invention relates to a polyacrylate functional polymer containing amino aromatic hydrocarbon structural units and a preparation method thereof, belonging to the technical field of polyacrylate functional polymers. Background technique [0002] As an important basic nutrient, vitamin B1 has many important physiological functions. The structural formula of vitamin B1 is as follows: [0003] [0004] As an important basic nutrient, vitamin B1 has many important physiological functions. In the past ten years, the preparation of vitamin B1 and its derivatives has attracted much attention. Among them, 2-methyl-4-amino-5-aminomethylpyrimidine is the key intermediate commonly used in the preparation of vitamin B1. And the present three kinds of routes about the synthesis of 2-methyl-4-amino-5-aminomethylpyrimidine all have various drawbacks: such as the cyanopyrimidine route needs to use a large amount of ethyl acetimide hydrochloride (1.8 to 2 equiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/34C08F2/38C07D239/42
Inventor 戚聿新陈军王涛王海涛鞠立柱李新发
Owner XINFA PHARMA
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