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Technique for synthesizing 2-hydroxy-5-tert octyl acetophenone

A technology of tert-octylacetophenone and process method is applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc. The effect of high yield, high product purity and simple post-processing

Inactive Publication Date: 2012-10-17
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In this process, dry HCl gas needs to be fed in, and the operation safety is low, and the discharge of waste gas and waste water is large.

Method used

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  • Technique for synthesizing 2-hydroxy-5-tert octyl acetophenone
  • Technique for synthesizing 2-hydroxy-5-tert octyl acetophenone
  • Technique for synthesizing 2-hydroxy-5-tert octyl acetophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 10.3g of 4-tertoctylphenol (0.05mol) and 30ml of tetrachloroethane into a 250ml four-necked flask equipped with a reflux device (attached with a drying device), a hydrogen chloride absorption device, and a mechanical stirring device, stir, and slowly add 7.9 g (0.1mol) acetyl chloride mixed with 25mL tetrachloroethane solution. After the dropwise addition, the temperature of the system was raised to 80° C., and the stirring was continued, and the reaction was kept for 2 hours, and the color of the solution changed from reddish brown to amber. At this temperature, add anhydrous aluminum chloride (8.1 g in total, 0.06 mol) in batches to the reaction solution, and finish adding in 1 hour. After the aluminum chloride is completely dissolved, add 1 g of acetyl chloride and mix with 3 mL of tetrachloroethane. The temperature of the solution was raised to 110° C., and the reaction was maintained for 10 hours. After the reaction is over, lower the temperature of the reacti...

Embodiment 2

[0031] Add 10.3g of 4-tertoctylphenol (0.05mol) and 30ml of nitrobenzene into a 250ml three-neck flask with a reflux device (attached with a drying device) and a mechanical stirring device, stir, and slowly add 10.2g (0.1mol) of acetic acid Anhydride and 30mL nitrobenzene mixed solution. After the dropwise addition was completed, the temperature of the system was raised to 90° C., the stirring was continued, and the reaction was kept for 3 hours. The color of the solution changed from reddish brown to amber. At this temperature, add anhydrous zinc chloride (total 7.7g, 0.057mol) in batches to the reaction solution, and finish the addition in 1 hour. After the zinc chloride is completely dissolved, add a mixed solution of 2 g of acetic anhydride and 4 mL of nitrobenzene , the temperature was raised to 105° C., and the reaction was maintained for 6 hours. After the reaction is over, lower the temperature of the reaction solution to room temperature, transfer it to a separatory ...

Embodiment 3

[0033]Add 10.3g of octylphenol (0.05mol) and 30ml of tetrachlorethylene into a 250ml four-necked flask equipped with a reflux device (attached with a drying device), a hydrogen chloride absorption device, and a mechanical stirring device, stir, and slowly add 7.9g (0.1mol ) Mixed solution of acetyl chloride and 25mL tetrachloroethylene. After the dropwise addition, the temperature of the system was raised to 80° C., and the stirring was continued, and the reaction was kept for 2 hours, and the color of the solution changed from reddish brown to amber. At this temperature, titanium tetrachloride liquid (total 11.4g, 0.06mol) was slowly added dropwise to the reaction solution, and after 1 hour, the mixed solution of 1g acetyl chloride and 3mL tetrachloroethylene was added, and the temperature was raised to 110°C, and the temperature was kept React for 10 hours. After the reaction, the temperature of the reaction solution was lowered to room temperature, added 50ml of 0.5mol / L h...

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Abstract

The invention discloses a technique for synthesizing 2-hydroxy-5-tert octyl acetophenone, belonging to the field of organic chemistry synthesis, characterized by using Fries rearrangement reaction of octylphenyl esters to synthesize 2-hydroxy-5-tert octyl acetophenone. The application of oximation products of the synthesized 2-hydroxy-5-tert octyl acetophenone by the technique as a copper extractant can raise the purity of copper and reduce the discharge amount of waste acid in wet copper smelting process. According to the invention, few by-product is produced in the process, there is no need for high temperature vacuum distillation and other purification steps, only acidification, washing and the like are needed, thus by the technique in 2-hydroxy-5-tert octyl acetophenone, the product has high purity and high yield, and the post-treatment is simple.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a process for synthesizing 2-hydroxy-5-tertoctylacetophenone. Background technique [0002] 2-Hydroxy-5-alkylacetophenone is a key intermediate in the synthesis of copper extractant 2-hydroxy-5-alkylacetophenone oxime, which is widely used in copper hydrometallurgical processes, such as currently in Lix973N and lix984N, which are widely used in the extraction and purification of copper all over the world, are composed of 5-nonyl salicylaldoxime and 2-hydroxy-5-nonylacetophenone oxime in a certain proportion, of which 2-hydroxy -5-Nonylacetophenone oxime can significantly improve the phase separation effect of the extraction process, the stripping performance of aldoxime, and improve the separation coefficient of copper and iron (references: H.AMINIAN, C.BAZIN, TECHNICAL NOTE: SOLVENT EXTRACTION EQUILIBRIA IN COPPER(II)-IRON(III)-LIX984SYSTEM, Miner...

Claims

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Application Information

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IPC IPC(8): C07C49/245C07C45/51
Inventor 李林艳徐晓庆蔡妍徐盛明
Owner TSINGHUA UNIV
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