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Functional polymer containing amino aryl ethylene and preparation method of functional polymer

A technology of aminoaromatic ethylene and aromatic vinyl, which is applied in the field of functional polymers of aminoaromatic ethylene and its preparation, can solve problems such as difficulty in removing o-chloroaniline, unfavorable environmental protection, long reaction cycle, etc., and achieve environmental protection Effects of industrial application, ease of industrial application, and raw material cost advantages

Active Publication Date: 2013-06-05
XINFA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the three kinds of routes about the synthesis of 2-methyl-4-amino-5-aminomethylpyrimidine all have various disadvantages: such as the cyanopyrimidine route needs to use a large amount of ethyl acetimide hydrochloride (1.8 to 2 Equivalent), 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; The formylaminopyrimidine route uses 3-aminopropionitrile as the 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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  • Functional polymer containing amino aryl ethylene and preparation method of functional polymer
  • Functional polymer containing amino aryl ethylene and preparation method of functional polymer
  • Functional polymer containing amino aryl ethylene and preparation method of functional polymer

Examples

Experimental program
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Effect test

Embodiment 1

[0052]Add 400 grams of ethanol, 100 grams of deionized water, and 80.5 grams (0.5 moles) of 2-acetamidostyrene into a 1000 milliliter stainless steel reactor; 1 g of ethanol solution, after dropping, heat up to an internal temperature of 115°C to 120°C, react for 3 hours, and the pressure at this time is 4-5 atmospheres; cool to an internal temperature of 80-85°C, add 0.8 g of dodecyl mercaptan , heat preservation reaction for 2 hours; filter while hot to remove a small amount of high molecular weight polymer; cool the filtrate to 50 degrees, add 100 grams of 25wt% sodium hydroxide aqueous solution, heat to 95-100 ° C for 4 hours; cool to 20 ° C, Filtrate and dry to obtain 56.5 g of solid poly-2-aminostyrene formula (1). The appearance is off-white solid particles, insoluble in cold water, slightly soluble in hot water, soluble in hot alcohol, and the yield is 95.0%.

Embodiment 2

[0054] 80.5 grams of 4-acetamidostyrene was used as a monomer to replace 2-acetamidostyrene in Example 1 for free radical polymerization. The specific reaction process was the same as in Example 1. The polymer yield is shown in Table 1.

Embodiment 3

[0056] 80.5 grams of 3-acetamidostyrene was used as a monomer to replace 2-acetamidostyrene in Example 1 for free radical polymerization. The specific reaction process was the same as in Example 1. The polymer yield is shown in Table 1.

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Abstract

The invention relates to a functional polymer containing amino aryl ethylene and a preparation method of the functional polymer. The preparation method comprises the following steps of: initiating free radical polymerization of a monomer acetamino aryl ethylene in an alcohol-water solvent by using a method for initiating solution polymerization by utilizing free radicals; then, adjusting the molecular weight of the polymer by using lauryl mercaptan; and separating in an alcohol-water system to obtain the functional polymer containing amino aryl ethylene, wherein the molecular weight of the functional polymer is within a certain range. The polymer can be dissolved or most of the polymer can be dissolved in the hot alcohol-water system; and the polymer can be used for substituting for highly-cancerogenic o-chloroaniline or other micromolecular aniline derivatives to prepare a key intermediate 2-methyl-4-amino-5-aminomethyl pyrimidine of vitamin B1. The functional polymer containing amino aryl ethylene can be recycled after being filtered; the polymer can be used for completely substituting for o-chloroaniline to prepare vitamin B1; and the preparation method is simple and convenient to operate and high in yield.

Description

technical field [0001] The invention relates to an aminoaromatic vinyl functional polymer and a preparation method thereof, belonging to the technical field of vinyl 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] 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 three kinds of routes about the synthesis of 2-methyl-4-amino-5-aminomethylpyrimidine all have various disadvantages: such as the cyanopyrimidine route needs to use a large amount of ethyl acetimide hydrochloride (1.8 to 2 Equivalent), the raw material and malononitrile are expensive, which is not conducive to the reduction of product cost; the reaction steps of the formy...

Claims

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Application Information

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IPC IPC(8): C08F112/14C08F126/06C08F2/04C08F2/38
Inventor 戚聿新成鹏飞陈军王涛王海涛鞠立柱李新发
Owner XINFA PHARMA
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