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N-bis (1-ethyl-propyl)-3-pentylamine and preparation method thereof

A technology of pentylamine and ethyl, which is applied in the field of N-bis-3-pentylamine and its preparation, can solve the problems of troublesome post-processing, slow reaction speed, and many reaction steps, etc., and achieve simple post-processing and reduce synthesis Cost, the effect of simplifying the reaction steps

Pending Publication Date: 2022-05-06
绍兴贝斯美化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that there are many reaction steps for the product, the post-treatment process is troublesome, and a large amount of sodium salt wastewater will be generated.
[0005] Literature (Chemistry-A European Journal (2013), 19 (11), 3665-3675) reports that 3-pentanol and 3-pentylamine are used as raw materials to synthesize the material by dehydration condensation of catalyst NiCuFeOx. The shortcoming of this method is that the catalyst The preparation process is cumbersome
[0006] The patent No. DE2527113A1 discloses the preparation of N,N-bis(α-ethylpropyl)benzamide and herbicides containing them, using 3-bromopentane and 3-aminopentane in alkali The material is synthesized by reacting under conditions, the disadvantage of this method is that the reaction speed is slow and the time required is long
[0007] Generally speaking, the preparation method of N-bis(1-ethyl-propyl)-3-pentylamine in the prior art has the defects of inconvenient operation and difficult post-treatment purification, which is not conducive to simple synthesis

Method used

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  • N-bis (1-ethyl-propyl)-3-pentylamine and preparation method thereof
  • N-bis (1-ethyl-propyl)-3-pentylamine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 10g of 3-pentanamine and 30mL of 3-pentanone (3-pentanone as a solution) into the autoclave, add 2g of p-toluenesulfonic acid and 2g of Pb / C, replace with nitrogen for 3 times, replace with hydrogen for 3 times, keep 0.8MPa Press for 20 minutes, turn on the stirrer, slowly raise the temperature to 80°C, control the pressure to 1.2MPa, GC sampling and analysis, if the raw material 3-amylamine ≤ 1%, stop the reaction, stop the introduction of hydrogen, cool down to 40°C, release the pressure, and then Nitrogen was replaced 3 times, the reaction liquid was heated and filtered, and the filtrate was distilled under reduced pressure in a rectification device to obtain 16.5 g of the product with a content of 99.1% and a yield of 91.5%.

Embodiment 2

[0039] Add 50g of 3-pentanamine and 150mL of 3-pentanone (3-pentanone as a solution) into the autoclave, add 2g of p-toluenesulfonic acid and 2g of Pb / C, replace with nitrogen for 3 times, replace with hydrogen for 3 times, keep 0.8MPa Press for 20 minutes, turn on the stirrer, slowly raise the temperature to 80°C, control the pressure at 1.2MPa, keep the temperature for 5 hours, and conduct sampling analysis by GC. If the raw material 3-amylamine ≤ 1%, stop the reaction, stop the hydrogen supply, and cool down to 40°C. The pressure was released, and then replaced with nitrogen for 3 times, the reaction liquid was heated and filtered, and the filtrate was distilled under reduced pressure in a rectification device to obtain 83.1 g of the product with a content of 99.0% and a yield of 92.0%.

Embodiment 3

[0041] Add 600g of 3-pentanamine and 1800mL of 3-pentanone (3-pentanone as a solution) into the autoclave, add 10g of p-toluenesulfonic acid and 10g of Pb / C, replace with nitrogen 3 times, replace with hydrogen 3 times, keep 0.8MPa Press for 20 minutes, turn on the stirrer, slowly raise the temperature to 80°C, control the pressure to 1.2MPa, react for 5h, GC sampling analysis, if the raw material 3-amylamine ≤ 1%, stop the reaction, stop the hydrogen supply, cool down to 40°C, and release pressure, then replaced with nitrogen for 3 times, the reaction solution was heated and filtered, and the filtrate was distilled under reduced pressure in a rectification device to obtain 994.5 g of the product, with a GC normalized content of 99.0% and a yield of 91.8%.

[0042] Analysis example

[0043] For gas chromatography analysis, a GC column equipped with HP-5 manufactured by Agilent Corporation and a 7820A GC analysis device manufactured by Agilent Corporation were used. For temper...

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Abstract

The invention discloses a preparation method of N-bis (1-ethyl-propyl)-3-pentylamine, which is characterized in that 3-pentylamine and 3-pentanone are directly adopted as raw materials, and under the simultaneous catalysis of hydrogen, a hydrogenation catalyst and an acid catalyst, the N-bis (1-ethyl-propyl)-3-pentylamine is synthesized by one-step reductive ammoniation. The method is short in reaction time, simple in post-treatment process, high in product yield and low in wastewater amount, the reaction steps are simplified, and the synthesis cost is reduced. According to the method, the N-bis (1-ethyl-propyl)-3-pentylamine can be prepared by a one-step method, and the obtained product is relatively few in impurities and relatively high in yield. The invention also provides a method for analyzing the N-bis (1-ethyl-propyl)-3-pentylamine and the raw material by using gas chromatography.

Description

technical field [0001] The invention belongs to the preparation method of fatty amine, in particular to N-bis(1-ethyl-propyl)-3-pentylamine and its preparation method. Background technique [0002] N-bis(1-ethyl-propyl)-3-pentylamine is a high-end fine chemical, which can be used as a lubricant for fuel oil and as a herbicide in the synthesis of pesticides with a mother core structure. [0003] The Chinese patent with the patent number CN101302168A discloses a method for preparing N-(1-ethylpropyl)-3,4-dimethylaniline, which belongs to the technical field of dinitroaniline pesticides, and its technical points are as follows: Ortho-xylene is used as the starting material, which is first nitrated under the action of a catalyst to obtain 3,4-dimethylnitrobenzene, and then hydrogenated with 3-pentanone under the action of a catalyst, added, and then hydrogenated to obtain N-( 1-ethylpropyl)-3,4-dimethylaniline. The N-(1-ethylpropyl)-3,4-dimethylaniline content of the invention...

Claims

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Application Information

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IPC IPC(8): C07C211/07C07C209/26
CPCC07C209/26C07C211/07
Inventor 田园陈湘朋倪丽囡颜谭
Owner 绍兴贝斯美化工股份有限公司
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