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Synthesis method of 5-amino-2, 4-dibromophenol

A technology of dibromophenol and synthesis method, applied in the preparation of amino hydroxy compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as unfavorable industrial production, difficult control of bromination in photocatalytic reaction, and achieve product yield High, high product purity, environmentally friendly effect

Pending Publication Date: 2022-04-12
棓诺(苏州)新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the photocatalytic reaction is not easy to control the position of bromination, and it is easy to obtain a mixture, which is not conducive to industrial production

Method used

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  • Synthesis method of 5-amino-2, 4-dibromophenol
  • Synthesis method of 5-amino-2, 4-dibromophenol
  • Synthesis method of 5-amino-2, 4-dibromophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1, a synthetic method of 5-amino-2,4-dibromobenzol, inter-aminophenol as a raw material, sequentially:

[0042]

[0043] (1) 0.138 mol (about 15.14 g) of amino phenol was added to 100 ml of reaction flask, and 60 ml of methanol was added (i.e., so that amino phenol was dissolved); stirring was lowered to -5 ° C, and the acetic anhydride was added dropwise. 0.166 mol (about 16.99g); temperature control is at -5 ~ 5 ° C, 0.5H dropcard; temperature control at 0 ° C for 2 h, at this time, the sampling point plate determines the reactance of the feedstock;

[0044]The resulting reaction solution was added to 20 ml of ice water, stirred at 0.5 h, 0 ° C to filter, and the resulting filter cake was 11 (2 * 80 mL), dried (at 50 ° C to constant weight), Acetamide-based phenol 18 g (about 0.12 mol), yield is about 87%.

[0045] (2) Dichloromethane and methanol were mixed according to the volume ratio of 5: 2, and the mixture of dichloromethane / methanol was mixed;

[0046] ...

Embodiment 2

[0050] Example 2, a synthetic method of 5-amino-2,4-dibromobenzol, inter-aminophenol as a raw material, sequentially:

[0051] (1) 0.276 mol (approximately 30.28 g) was added to 200 ml of reaction flask (about 30.28 g), and 120 ml of methanol was added, and the mixture was stirred down to -5 ° C, and 0.332 mol (about 34 g) of acetic anhydride was started. -5 ~ 5 ° C, 0.5H dropcard; temperature control at 0 ° C for 2 h, at this time, the sampling point plate determines the reactance of the feedstock;

[0052] The resulting reaction solution was added to ice water (about 40 mL), stirred for 0.5 h, filtration (0 ° C) to give filter cake, ice water twice, dry, greased acetamine phenol 35 g, yield of about 83% .

[0053] (2) Dichloromethane and methanol were mixed according to the volume ratio of 5: 2, and the mixture of dichloromethane / methanol was mixed;

[0054] The metalloacethane-based phenol 12g was administered in a 200 ml reaction bottle, and 120 ml of dichloromethane / metha...

Embodiment 3

[0059] Example 3, a synthetic method of 5-amino-2,4-dibromobenzol, inter-aminophenol as a raw material, specifically the following steps:

[0060] (1) Add a 10 L reaction vessel 13.87 mol (about 1514 g), and then adding methanol 6L to stir well; stirring and cooling to -5 ° C to start dropping acetic anhydride 16.64 mol; temperature control at -5 ~ 5 ° C, 2H is added; the temperature control is at 0 ° C for 2 h, and the sampling point plate determines the reactance of the feedstock;

[0061] The reaction mixture was added to ice water (about 2 L), stirred for 0.5 h, filtration (0 ° C) to give filter cake, ice water twice, dry degree acetamide-based phenol 1.9 kg, yield of about 90.7%.

[0062] (2) Dichloromethane and methanol were mixed according to the volume ratio of 5: 2, and the mixture of dichloromethane / methanol was mixed;

[0063] The sputum-based phenol was put into 10 l (about 600 g) in a 10 L reaction bottle, and the mixture was stirred with dichloromethane / methanol ...

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PUM

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Abstract

The invention discloses a synthesis method of 5-amino-2, 4-dibromophenol, which takes m-aminophenol as a raw material and comprises the following steps: dissolving m-aminophenol in an organic solvent, and dropwise adding anhydride for reaction; dissolving the obtained m-amide phenol in an organic mixed solvent, and then adding a bromination reagent for reaction; and adding alcohol and hydrochloric acid into the obtained 2, 4-dibromo-5-amide phenol, stirring, refluxing and reacting until the solution is clear, and carrying out post-treatment on the reaction solution to obtain the product 5-amino-2, 4-dibromophenol. The raw materials are cheap and easy to obtain; the reaction conditions are simple and mild; the yield is high; the target product quality is high.

Description

Technical field [0001] The invention belongs to the field of organic luminescent materials, and more particularly to a synthesis method of 5-amino-2,4-dibromobenophenol. Background technique [0002] In recent years, organic small molecules have been widely used as new materials in the field of organic electroluminescence, airport effect transistors, organic solar cell energy. An organic electroluminescence is advantageous for new display technologies with low cost, light weight, flexibility, and other advantages, which has been mature, in electron end products to widespread applications. However, there are still many problems in the industrialization process, such as the luminous efficiency and service life of the device. Phenol derivatives have good thermal stability and light performance, structurally easily modified and can form uniform, stable amorphous film, which is often used to construct fluorescent materials and structural units of the device, so relevant research on ne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C215/76
Inventor 吴清来宋文志李显跃杨雪
Owner 棓诺(苏州)新材料有限公司
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