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Synthesizing method for 9,10-dimethylanthracene

A technology of dimethyl anthracene and synthetic method, which is applied in 9 fields, and achieves the effects of low preparation cost, less by-products and high purity

Inactive Publication Date: 2016-03-09
高大元
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And for 9,10-dimethyl anthracene research papers and synthetic methods have not been reported, therefore, can develop a kind of high purity, low cost, synthetic simple 9,10-dimethyl anthracene synthetic method, to The development of related fields is of great significance

Method used

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  • Synthesizing method for 9,10-dimethylanthracene

Examples

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Effect test

example 1

[0015] Firstly, put 30mL of o-xylene into the reaction kettle, add 0.5g of manganese acetate, 15mL of acetic acid and 10mL of paraldehyde into it respectively, and react for 2 hours at a temperature of 210°C and a pressure of 2.5MPa. After the reaction is completed, , placed in a centrifuge for centrifugal separation, and dried to obtain crude phthalic acid; then, under the conditions of controlling the temperature at 280°C and the pressure at 6.5MPa, dissolve the crude phthalic acid obtained above in 30mL of water, and then add 1g of sodium bromide , pass through hydrogen to react for 1 hour, after the reaction is completed, place in ice water for 8 minutes, filter, wash once with water, dry to obtain fine phthalic acid, and set aside; then take 30mL of o-xylene into the reaction container, pour it into Add 10mL of liquid bromine and 1g of iron powder respectively, control the temperature at 350°C and rotate at 700r / min, stir magnetically for 40min, after the stirring is compl...

example 2

[0017] Firstly, put 32mL o-xylene into the reaction kettle, add 0.7g manganese acetate, 18mL acetic acid and 12mL paraldehyde to it, and react for 2.5h at a temperature of 220°C and a pressure of 2.8MPa until the reaction is complete Afterwards, put it in a centrifuge for centrifugation and dry to obtain the crude phthalic acid; then, under the conditions of controlling the temperature at 285°C and the pressure at 6.7MPa, dissolve the crude phthalic acid obtained above in 35mL of water, and then add 1.1g of bromine Sodium chloride, add hydrogen to react for 1.5h, after the reaction is completed, place in ice water for 9min, filter, wash twice with water, dry to obtain fine phthalic acid, set aside; then take 32mL o-xylene and put it into the reaction container , add 13mL of liquid bromine and 1.5g of iron powder to it respectively, control the temperature at 360°C and rotate at 800r / min, stir magnetically for 45min, after the stirring is completed, cool down to 75°C at a speed ...

example 3

[0020]Firstly, put 35mL of o-xylene into the reaction kettle, add 0.9g of manganese acetate, 20mL of acetic acid and 14mL of paraldehyde respectively, and react for 3 hours at a temperature of 230°C and a pressure of 3.0MPa. After the reaction is completed, , placed in a centrifuge for centrifugal separation, and dried to obtain crude phthalic acid; then, under the conditions of controlling the temperature at 290°C and the pressure at 6.9MPa, dissolve the crude phthalic acid obtained above in 40mL of water, and then add 1.2g bromide sodium, and hydrogen gas was introduced to react for 2 hours. After the reaction was completed, put it in ice water for 10 minutes, filter it, wash it twice with clean water, and dry it to obtain fine phthalic acid. Add 15mL of liquid bromine and 2g of iron powder respectively, control the temperature at 370°C and rotate at 900r / min, stir magnetically for 50min, after the stirring is completed, cool down to 80°C at a speed of 15°C / min, react for 2h,...

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Abstract

The invention discloses a synthesizing method for 9,10-dimethylanthracene, and belongs to the technical field of chemical synthesis. The method comprises the steps that o-xylene is taken as raw materials, under the action of a manganese acetate catalyst and a paraldehyde accelerant, acetic acid is added, and the materials are mixed and react; after centrifugal separation is performed, a mixture obtained in the last step is dissolved in water under the certain pressure, a sodium bromide catalyst is added, and after hydrogen gas is introduced for a reaction, filtering, washing and drying are performed to obtain phthalic acid; o-xylene is taken again, liquid bromine and iron powder are added to be mixed with the o-xylene, the temperature is lowered for a reaction, after cooling is performed, magnesium powder and glutamyl transpeptidase are added, and sealed preservation and enzymolysis are performed; a product obtained in the last step is taken out to be dried, the prepared phthalic acid is added, acetic acid and concentrated sulfuric acid are added, the materials are mixed and react, standing and filtering are performed, and drying is performed to obtain the 9,10-dimethylanthracene. The synthesizing method has the advantages that the synthesizing steps are simple, the preparation cost is low, by-products obtained in the synthesizing process are few, the obtained 9,10-dimethylanthracene is high in purity, and the yield reaches 94.5% or above.

Description

technical field [0001] The invention relates to a method for synthesizing 9,10-dimethylanthracene, which belongs to the technical field of chemical synthesis. Background technique [0002] Anthracene is also called scintillation crystal, a condensed ring aromatic hydrocarbon containing three rings. A triphenyl ring composed of solid polycyclic aromatic hydrocarbons. It is found in coal tar. The centers of the three rings of anthracene are on a straight line and are isomers of phenanthrene. Anthracene is a colorless flaky crystal with blue-purple fluorescence and easy sublimation; it is insoluble in water, hardly soluble in ethanol and ether, and easily soluble in hot benzene. The chemical activity of 9 and 10 positions in anthracene molecule is relatively high, and it can be oxidized with nitric acid to generate 9,10-anthraquinone (see anthraquinone for the structural formula), which is an important intermediate for the synthesis of anthraquinone dyes; it can be reduced w...

Claims

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Application Information

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IPC IPC(8): C12P15/00C07C15/28
CPCC12P15/00C07C1/326
Inventor 高大元盛艳花
Owner 高大元
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