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Preparation method of dibromine naphthalene

A dibromonaphthalene and liquid bromine technology, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of low reaction temperature and long reaction time, and achieve high yield and high economy of reaction atoms Effect

Inactive Publication Date: 2007-03-07
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method also has many shortcomings, such as long reaction time, the reaction time is two days; the reaction temperature is low, the reaction temperature is -30 ℃; the volatile organic solvent dichloromethane is used in the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The first step, put 0.4mmol naphthalene and 1.2800g OMImBr ionic liquid into the closed reactor, add 5.1200g 1.0mol / l sulfuric acid at the same time, stir and mix evenly, then add 0.1ml of liquid bromine;

[0017] The second step is to seal the airtight reactor treated in the first step and place it in a water bath with a temperature of 60°C for constant temperature reaction for 6 hours, take out the airtight reactor, open it after natural cooling, and extract it with benzene;

[0018] The third step is to add toluene reference substance in the solution obtained after benzene treatment, and carry out gas chromatographic analysis. Yield up to 90% (in terms of naphthalene).

[0019] In the fourth step, the benzene is re-used by rotary evaporation, and the bottom liquid after extraction can be recycled, and the yield of the target product can reach more than 80% (calculated by naphthalene).

Embodiment 2

[0021] The first step, put 0.4mmol naphthalene and 1.0240g DMImBr ionic liquid into a closed reactor, add 0.5120g 3.0mol / l sulfuric acid at the same time, stir and mix evenly, then add 0.15ml of liquid bromine;

[0022] The second step is to seal the airtight reactor treated in the first step and place it in a water bath with a temperature of 80°C for 9 hours of constant temperature reaction, take out the airtight reactor, open it after natural cooling, and extract it with petroleum ether;

[0023] The third step, adding toluene reference substance in the solution obtained after petroleum ether treatment, carries out gas chromatographic analysis. Yield up to 90% (in terms of naphthalene).

[0024] In the fourth step, the petroleum ether is re-used by rotary evaporation, and the bottom liquid after extraction can be recycled, and the yield of the target product can reach more than 80% (calculated by naphthalene).

Embodiment 3

[0026] The first step, put 0.4mmol naphthalene and 1.5360gBMIm PF6 ionic liquid into the closed reactor, add 5.1200g 4.0mol / l sulfuric acid at the same time, stir and mix evenly, then add 0.15ml of liquid bromine;

[0027] The second step is to seal the airtight reactor treated in the first step and place it in a water bath with a temperature of 90° C. for constant temperature reaction for 12 hours, take out the airtight reactor, open it after natural cooling, and extract it with acetone;

[0028] The 3rd step, in the solution gained after acetone treatment, add toluene standard substance, carry out gas chromatographic analysis. Yield up to 90% (in terms of naphthalene).

[0029] In the fourth step, the acetone is re-used by rotary evaporation, and the bottom liquid after extraction can be recycled, and the yield of the target product can reach more than 80% (calculated by naphthalene).

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Abstract

The invention discloses a catalyzing synthesizing method of naphthalene dibromide in the organic chemical synthetic technological domain, which is characterized by the following: making naphthalene as raw material; adopting liquid bromine as bromine source; making sulphuric acid and ionic liquid with imidazole ring cation as solvent; reacting in the sealed reactor to produce the product.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing dibromonaphthalene, specifically, a method for catalytically synthesizing dibromonaphthalene from naphthalene and bromine, and belongs to the technical field of organic chemical synthesis. Background technique [0002] Dibromonaphthalene is an important intermediate in organic synthesis, and it has attracted attention in recent years because of its phosphorescent properties. Although it has many potential application values, its production technology is very backward at present, the market demand is small and the sales price is high. The traditional method for synthesizing dibromonaphthalene is that people such as ROBERTW.RAYER disclose a kind of method for preparing dibromonaphthalene in the 23rd phase 311 page of " J.Org.Chem " (1958), promptly adopt naphthalene as raw material, with Dioxane is used as a solvent and prepared by adding liquid bromine. The yield ...

Claims

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Application Information

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IPC IPC(8): C07C25/22C07C17/12
CPCY02P20/54
Inventor 单永奎赵新华顾颖颖
Owner EAST CHINA NORMAL UNIVERSITY
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