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Method for selectively synthesizing N-alkylaminopropionate solution

An alkylaminopropionate, selective technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc. The effect of reducing entrainment and avoiding aggregation

Active Publication Date: 2020-10-30
WENZHOU INST UNIV OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the reaction, the excess of acrylate is 10-30%. Raising the reaction temperature to 60-120 degrees is beneficial to obtain the maximum proportion of the mono-addition product N-alkylalanine / ester / salt, but this method, except for the unavoidable In addition to diacrylate addition products, N-alkylaminopropionamide, a by-product of acrylate amination, will also be obtained
U.S. Patent No. 5,922,909 introduces a method for adjusting the ratio of N-alkylaminopropionate and N-alkylaminodipropionate by controlling the pH of the reaction. Absolute advantage
Therefore, existing synthetic method is difficult to obtain N-alkyl amino propionate alone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for selectively synthesizing N-alkylaminopropionate solution, comprising the following steps:

[0030] S1: Using dodecylamine and methyl acrylate as raw materials, add 43 grams of methyl acrylate (0.5 mol) dropwise to 186 grams of dodecylamine (1.0 mol), dropwise for 1.5 hours, and then react at 30°C for 18 hours; the whole process is accompanied by stirring, and the stirring speed is 120 rpm;

[0031] S2: Add 600 milliliters of 1.0 mol / liter potassium hydroxide aqueous solution to the reaction solution, react at 25°C for 18 hours, and the solution turns from the initial cloudy state to translucent state;

[0032] S3: Add 2.5 liters of pure water to the reaction solution, add 0.8 liters of ethyl acetate to extract the reaction solution, and extract a total of 3 times;

[0033] S4: Collect the ethyl acetate layer, recover ethyl acetate and dodecylamine; the obtained aqueous layer solution is distilled to 800 grams at 50°C and a pressure of 0.02MPa, and the cont...

Embodiment 2

[0035] A method for selectively synthesizing N-alkylaminopropionate solution, comprising the following steps:

[0036] S1: Using dodecylamine and methyl acrylate as raw materials, add 43 g of methyl acrylate (0.5 mol) dropwise to 372 g of dodecylamine (2.0 mol), drop it in 2.0 hours, and then react at 75°C for 12 Hour; the whole process is accompanied by stirring, and the stirring speed is 150 rev / min;

[0037] S2: Add 500 ml of 2.0 mol / L potassium hydroxide aqueous solution to the reaction solution, and react at 70°C for 10 hours, the solution turns from the initial turbid state to translucent;

[0038] S3: Add 6.0 liters of pure water to the reaction solution, add 2.0 liters of ethyl acetate to extract the reaction solution, and extract twice in total;

[0039] S4: Collect the ethyl acetate layer, recover ethyl acetate and dodecylamine; the obtained aqueous layer solution is distilled to 800 grams at 70°C and a pressure of 0.03MPa, and the content of potassium N-alkylalanin...

Embodiment 3

[0041] A method for selectively synthesizing N-alkylaminopropionate solution, comprising the following steps:

[0042] S1: Using dodecylamine and methyl acrylate as raw materials, add 43 g of methyl acrylate (0.5 mol) dropwise to 140 g of dodecylamine (0.75 mol), dropwise for 1.0 hour, and then react at 30°C for 12 hours; the whole process is accompanied by stirring, and the stirring speed is 80 rpm;

[0043] S2: Add 1000 ml of 0.5 mol / L potassium hydroxide aqueous solution to the reaction solution, and react at 25°C for 10 hours, the solution turns from the initial cloudy state to translucent state;

[0044] S3: Add 1.0 liter of pure water to the reaction solution, add 300 ml of ethyl acetate to extract the reaction solution, and extract 3 times in total;

[0045] S4: Collect the ethyl acetate layer, recover ethyl acetate and dodecylamine; the obtained aqueous layer solution is distilled to 800 grams at 35°C and a pressure of 0.01MPa, and the content of potassium N-alkylalan...

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Abstract

The invention belongs to the technical field of organic synthesis and particularly discloses a method for selectively synthesizing an N-alkylaminopropionate solution. The method comprises the following steps: with akyl primary amine and acrylate as raw materials, dropwise adding acrylate into excessive alkyl primary amine and carrying out stirring for a reaction to allow the reaction to be implemented in the direction of generating N-alkylamino propionic ester, then adding an aqueous solution of alkali metal hydroxide to convert N-alkylamino propionic ester into N-alkylaminopropionate, and removing excessive alkyl primary amine through extracting via an organic solvent, thereby realizing selective synthesis of N-alkylaminopropionate. According to the method, high-purity N-alkylaminopropionate can be obtained, and an impurity content can be reduced to 5% or below; high temperature, high pressure and complex crystallization and purification steps are not needed, so the method is simple and feasible; and the used raw materials and solvents can be recycled, so the method is very energy-saving and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for selectively synthesizing N-alkylaminopropionate solution. Background technique [0002] N-Alkylaminopropionates and N-Alkylaminodipropionates are two types of very useful surfactants, which are widely used as cleaning agents, emulsifiers, flotation agents and electroplating additives, etc. The synthesis of these two types of compounds is basically obtained by converting fatty amines and α, β-unsaturated acids, nitriles or esters under certain conditions, but the reaction products are mixed with N-alkylaminopropionate and N-alkylaminodipropyl However, due to the difference in the hydrophilic and lipophilic properties of N-alkylaminopropionate and N-alkylaminodipropionate and the wide application in daily chemicals such as household detergents and cosmetics, selective preparation is required Both types of substances are of high purity. [0003] ...

Claims

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Application Information

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IPC IPC(8): C07C227/06C07C229/12C07C227/40
CPCC07C227/06C07C227/40C07C229/12
Inventor 周华彭波谭颖
Owner WENZHOU INST UNIV OF CHINESE ACAD OF SCI
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