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Preparation of 3-(N-ethyl-N-isoamyl) amino phenol

A technology of ethylaminophenol and aminophenol, which is applied in the field of preparation of 3-aminophenol, can solve the problems of high production process cost, unfavorable industrial production, and low purity of EPA, and achieve the effects of low price, easy industrial production, and high purity

Active Publication Date: 2011-11-16
康爱特维迅(蓬莱)化学有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cost of this production process is relatively high, a catalyst needs to be added in the reaction process, the operation is complicated, and the purity of the obtained EPA is not high, which is not conducive to industrial production

Method used

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  • Preparation of 3-(N-ethyl-N-isoamyl) amino phenol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1, the preparation method of 3-(N-ethyl-N-isoamyl) aminophenol is that at room temperature, successively 77g resorcinol and 53g content are 65% monoethylamine aqueous solution to add 250ml In a high-pressure reactor, heat up to 165-175°C, keep warm until the reaction is over, transfer the material to a beaker when the temperature drops to 40°C after the reaction, and slowly add 80ml of 30% liquid caustic soda under stirring, that is, containing hydrogen Sodium 0.8mol, add 25g caustic soda after adding, continue to cool down to 0-10°C, filter to get about 160g of 3-ethylaminophenol sodium salt; add 50ml water into a 1000ml flask at room temperature, add 3-ethylaminophenol under stirring 160g of sodium phenolate, adjust the pH to 6-7 with industrial hydrochloric acid, then raise the temperature to 80°C, add 95g of isopentyl bromide dropwise, and keep it warm for reaction. About 100 g of the product 3-(N-ethyl-N-isoamyl)aminophenol was obtained, with a content o...

Embodiment 2

[0014] Embodiment 2, the preparation method of 3-(N-ethyl-N-isoamyl) aminophenol is at room temperature, successively 77g resorcinol and 58g content are 60% ethylamine aqueous solution to add 250ml high pressure In the reaction kettle, heat up to 180°C and keep warm until the reaction is over. When the material cools down to 30°C after the reaction, transfer it to a beaker, slowly add 100ml of 30% liquid caustic soda under stirring, and then add 30g of caustic soda , continue to cool down to 0-10°C, filter to obtain about 160g of 3-ethylaminophenol sodium salt; add 50ml of water into a 1000ml flask at room temperature, add 160g of the previous reaction product 3-ethylaminophenol sodium salt under stirring, and use industrial Adjust the pH to 6-7 with hydrochloric acid, then raise the temperature to 80°C, add 150g of bromoisopentane dropwise, and keep it warm for reaction. Ethyl-N-isoamyl)aminophenol is about 100g, and the content is more than 95.0%.

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Abstract

The invention discloses a preparation method for 3-(N-ethyl-N-isoamyl) aminophenol. An ethylamine aqueous solution is used for reacting with resorcinol to obtain 3-ethylamino phenol; the obtained 3-ethylamino phenol is added with industrial 30% sodium hydroxide aqueous solution and industrial solid sodium hydroxide to produce a sodium salt, and then added with industrial hydrochloric acid for acidification in order to obtain pure 3-ethylamino phenol; and the purified 3-ethylamino phenol reacts with isoamyl bromide to obtain 3-(N-ethyl-N-isoamyl) aminophenol. The preparation method is characterized by reaction raw materials with low prices, requiring no catalyst, intermediate product adopting the method of purifying by salt, simple operation, good crystallization state, high purity and being easy for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of 3-(N-ethyl-N-isoamyl)aminophenol. Background technique [0002] 3-(N-ethyl-N-isoamyl)aminophenol is a key intermediate for the synthesis of fluoran-based thermosensitive dye S205. The traditional synthesis process of this intermediate uses resorcinol and isoamylamine in the catalyst In the presence of the reaction, the product 3-isoamylaminophenol is ethylated after the reaction to obtain 3-(N-ethyl-N-isoamyl)aminophenol. However, the cost of this production process is relatively high, a catalyst needs to be added in the reaction process, the operation is complicated, and the purity of the obtained EPA is not high, which is not conducive to industrial production. Contents of the invention [0003] The object of the present invention is to improve the deficiencies of the prior art and provide a kind of 3-( The preparation method of N-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/76C07C213/08
Inventor 贺承相林淑美丛国日梁军包恩伟王万杰
Owner 康爱特维迅(蓬莱)化学有限公司
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