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Environment-friendly synthesis method of 1-naphthylamine

A technology of green synthesis and naphthylamine, applied in the preparation of amino groups replacing hydrogen atoms, organic chemistry, etc., can solve the problems of long process, high cost, environmental pollution, etc., and achieve the effect of short process, low cost and improved conversion efficiency

Active Publication Date: 2015-08-12
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The method for preparing 1-naphthylamine in the prior art has defects such as long process flow, environmental pollution, and high cost. The purpose of the present invention is to provide a method for preparing 1-naphthylamine with simple steps, low cost and environmental friendliness. Methods

Method used

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  • Environment-friendly synthesis method of 1-naphthylamine

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Experimental program
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Effect test

Embodiment 1

[0029] Take by weighing 2.5g of hydroxylamine hydrochloride, drop into the three-necked flask that is connected with thermometer, condenser tube, then measure 12mL glacial acetic acid and 3mL deionized water and join in the three-necked flask, then place the three-necked flask in a constant temperature water bath, at 30 After stirring at a constant temperature for 20 minutes at °C, 0.5 g of naphthalene was added, the temperature was raised to 80 °C, and the reaction was stopped after 12 hours of constant temperature reaction. After post-processing the reaction solution, 0.54 g of the final product was obtained. The mass of 1-naphthylamine in the product was quantitatively analyzed by liquid chromatography external standard method to be 14.5 mg, and the yield was 2.64%.

Embodiment 2

[0031] Take by weighing 2.5g of hydroxylamine hydrochloride, drop into the three-necked flask that is connected with thermometer, condenser tube, then measure 12mL glacial acetic acid and 3mL deionized water and join in the three-necked flask, then place the three-necked flask in a constant temperature water bath, at 30 After stirring at a constant temperature for 20 minutes at ℃, 0.5 g of naphthalene was added, the temperature was raised to 80 ℃, and the reaction was stopped after 24 hours of constant temperature reaction. After post-processing the reaction solution, 0.54 g of the final product was obtained. The quality of 1-naphthylamine in the product was quantitatively analyzed by liquid chromatography external standard method, and the yield was 8.09%.

[0032] Analysis from liquid chromatography figure 1 As can be seen in (b), the reaction generates 1-naphthylamine, wherein the retention time of 1-naphthylamine is about 6.4 minutes, and the retention time of raw material...

Embodiment 3

[0038] Weigh 0.025g of sodium metavanadate and 1.0g of hydroxylamine hydrochloride respectively, put them into a three-necked flask connected with a thermometer and a condenser tube, then measure 15mL of acetic acid and 5mL of deionized water into the three-necked flask, and then place the three-necked flask on In a constant temperature water bath, stir at 30°C for 20 minutes, then add 0.5 g of naphthalene, raise the temperature to 80°C, and stop the reaction after 2 hours of constant temperature reaction. After post-processing the reaction solution, 0.58 g of the final product was obtained. The mass of 1-naphthylamine in the product was quantitatively analyzed by liquid chromatography external standard method to be 61.5 mg, and the yield was 11%.

[0039] From Example 1, Example 2 and Example 3, it can be seen that the addition of the catalyst can obviously promote the reaction and improve the productive rate of 1-naphthylamine.

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Abstract

The invention discloses an environment-friendly synthesis method of 1-naphthylamine. The method is characterized in that in a mixed solvent of glacial acetic acid and water, naphthalene and hydroxylammonium salts carry out one-step reaction to generate 1-naphthylamine. The method is low in cost, simple in process, short in flow and mild in reaction conditions, is environment-friendly and meets the industrial production requirements.

Description

technical field [0001] The invention relates to a green synthesis method of 1-naphthylamine, which belongs to the field of organic synthesis. Background technique [0002] 1-Naphthylamine, also known as α-naphthylamine and menaphthylamine, is an intermediate for the production of direct dyes, acid dyes, ice dyes and disperse dyes, and is also the main raw material for various rubber antioxidants. 1-naphthol produced from -naphthylamine is an important intermediate of the pesticide carbaryl. [0003] The naphthalene nitration reduction method is the main preparation method of 1-naphthylamine. This method uses naphthalene as a raw material to obtain 1-nitronaphthalene through nitration, and then obtains 1-naphthylamine through reduction. In the traditional 1-naphthylamine production process, nitric acid-sulfuric acid mixed acid is used for nitration in the nitration section, and iron powder reduction method or alkali sulfide reduction method is used in the reduction section. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/58C07C209/02
Inventor 刘平乐熊伟郝芳王恺君罗和安
Owner XIANGTAN UNIV
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