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Synthesis method for N-(3-aminopropyl) methacrylamide hydrochloride

A technology of methacrylamide hydrochloride and methacryloylpropylenediamine, which is applied in the field of synthesis of N-methacrylamide hydrochloride and can solve the problem of N-(3-aminopropyl)methyl Acrylamide hydrochloride synthesis reports and other issues, to achieve the effect of high yield and low cost

Inactive Publication Date: 2013-07-17
甘肃科瑞生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the synthesis of N-(3-aminopropyl)methacrylamide hydrochloride in China

Method used

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  • Synthesis method for N-(3-aminopropyl) methacrylamide hydrochloride
  • Synthesis method for N-(3-aminopropyl) methacrylamide hydrochloride
  • Synthesis method for N-(3-aminopropyl) methacrylamide hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The synthetic method of N-(3-aminopropyl) methacrylamide hydrochloride,

[0029] first step:

[0030]

[0031] Dissolve 100 grams of propylenediamine in 1000 milliliters of ethyl acetate, lower the temperature to below 0°C, dissolve 147 grams of di-tert-butyl dicarbonate in 500 milliliters of ethyl acetate and add dropwise, and keep reacting during the dropping process liquid below 10°C. After the dropwise addition, the reaction was completed for 10 hours, and the reaction was detected by GC. Ethyl acetate was distilled off under normal pressure, excessive propylenediamine was distilled off under the circulating water pump, and then 50 grams of N-Boc-1.3-propylenediamine was distilled under the vacuum condition of 5mm / hg, yield 22%, GC Purity greater than 95% for the next reaction.

[0032] Step two:

[0033]

[0034] Dissolve 50 grams of N-Boc-1.3-propylenediamine prepared in the first step in 500 milliliters of ethyl acetate, add 34.8 grams of triethylamine,...

Embodiment 2

[0039] first step:

[0040]

[0041] Dissolve 100g of propylenediamine in 1000ml of ethyl acetate, cool down to below 0°C, dissolve 98g of di-tert-butyl dicarbonate in 330ml of ethyl acetate and add dropwise, keep the reaction solution at 10°C during the dropwise addition the following. After the dropwise addition, the reaction was completed for 10 hours, and the reaction was detected by GC. Ethyl acetate was distilled off under atmospheric pressure, excessive propylenediamine was distilled off under the circulating water pump, and then 47g of N-Boc-1.3-propylenediamine was distilled under vacuum conditions with a vacuum degree of 1mm / hg, the yield was 20%, and the GC purity was greater than 95% was used for the next reaction.

[0042] Step two:

[0043]

[0044] Dissolve 47g of N-Boc-1.3-propylenediamine prepared in the first step in 900ml of ethyl acetate, add 27g of triethylamine, lower the temperature below 0°C, add 28g of methacryloyl chloride dropwise, a...

Embodiment 3

[0049] first step:

[0050]

[0051] Dissolve 100g of propylenediamine in 1200ml of ethyl acetate, cool down to below 0°C, dissolve 294g of di-tert-butyl dicarbonate in 800ml of ethyl acetate and add dropwise, keep the reaction solution at 10°C during the dropwise addition the following. After the dropwise addition, the reaction was completed for 10 hours, and the reaction was detected by GC. Ethyl acetate was distilled off at normal pressure, excess propylenediamine was distilled off under the circulating water pump, and then 35g of N-Boc-1.3-propylenediamine was distilled under vacuum conditions with a vacuum degree of 600mm / hg, the yield was 15%, and the GC purity was greater than 95 % for the next reaction.

[0052] Step two:

[0053]

[0054] Dissolve 35g of N-Boc-1.3-propylenediamine prepared in the first step in 200ml of ethyl acetate, add 40g of triethylamine, lower the temperature below 0°C, add 31g of methacryloyl chloride dropwise, and keep the temp...

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Abstract

The invention discloses a synthesis method for N-(3-aminopropyl) methacrylamide hydrochloride. The synthesis method comprises the following steps of: taking propane diamine and methacryloyl chloride as reactants, taking ethyl acetate as a reaction medium, reacting in the presence of Boc amino, and then removing Boc, so as to obtain N-(3-aminopropyl) methacrylamide hydrochloride. The industrialized synthesis route for N-(3-aminopropyl) methacrylamide hydrochloride disclosed by the invention is low in cost and high in productivity. The obtained product is high in purity, wherein the purity of N-Boc-1,3-propane diamine in the first step is greater than 95%, the purity of N-Boc-methylacryloyl propane diamine in the second step is greater than 96%, and the purity of the final product in the third step is greater than 96%.

Description

technical field [0001] The invention relates to a synthesis method of N-(3-aminopropyl)methacrylamide hydrochloride, belonging to the field of organic synthesis. Background technique [0002] N-(3-aminopropyl)methacrylamide hydrochloride is a very important intermediate of medicine, pesticide and other chemical additives. However, there is no report on the synthesis of N-(3-aminopropyl)methacrylamide hydrochloride in China. Contents of the invention [0003] The technical problem to be solved by the present invention is to overcome the existing defects and provide a kind of N-(3-aminopropyl)methacrylic acid with low product cost, high yield and high synthetic purity, which is suitable for industrial production and application Synthetic method of amide hydrochloride. [0004] The purpose of the present invention is specifically achieved through the following technical solutions: [0005] A kind of synthetic method of N-(3-aminopropyl) methacrylamide hydrochloride, take p...

Claims

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Application Information

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IPC IPC(8): C07C233/38C07C231/12
Inventor 杨径李建东
Owner 甘肃科瑞生物科技有限公司
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