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Method for synthetizing 3, 3'-dimethyl-9, 9'-dianthranide

A synthesis method and dimethyl technology, applied in 3 fields, can solve the problems of many reaction steps, low reaction yield and the like

Inactive Publication Date: 2012-12-05
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the reaction yield of this method is lower, and reaction steps are more

Method used

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  • Method for synthetizing 3, 3'-dimethyl-9, 9'-dianthranide
  • Method for synthetizing 3, 3'-dimethyl-9, 9'-dianthranide
  • Method for synthetizing 3, 3'-dimethyl-9, 9'-dianthranide

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Experimental program
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Embodiment 1

[0031] Synthesis of 3,3'-Dimethyl-9,9'-Bianthracene

[0032] (1) Synthesis of 3-methylanthrone

[0033] Add 2-methylanthraquinone (0.1mol, 22.2g), tin particles (0.2mol, 23.8g) and 200mL of acetic acid into a 500mL three-neck flask. The amount of acetic acid added is not specifically limited, and it can dissolve 2-methylanthraquinone That's it. 60mL of 37% (mass) concentrated hydrochloric acid was added under stirring at a temperature of 20-25°C, heated to 130°C, and stirred at a temperature of 130°C for 2h. After cooling to 25°C, pour the reaction solution into 100mL of water, and solids precipitated out. The reaction solution was left to stand and filtered to obtain a filter cake. The filter cake was washed with 100mL of water until the washing liquid was neutral, and the filter cake was mixed with acetone and 120 mL of n-hexane mixed solvent was used for recrystallization. The volume ratio of acetone to n-hexane in the mixed solvent used was 1:3 to obtain 15.1 g of 3-meth...

Embodiment 2

[0047] (1) Synthesis of 3-methylanthrone

[0048]Add 2-methylanthraquinone (0.1mol, 22.2g), tin particles (0.2mol, 23.8g) and 200mL of acetic acid into a 500mL three-neck flask. The amount of acetic acid added is not specifically limited, and it can dissolve 2-methylanthraquinone That's it. 60mL of 37% (mass) concentrated hydrochloric acid was added under stirring at a temperature of 20-25°C, heated to 130°C, and stirred at a temperature of 130°C for 2h. After cooling to 25°C, pour the reaction solution into 100mL of water, and solids precipitated out. The reaction solution was left to stand and filtered to obtain a filter cake. The filter cake was washed with 100mL of water until the washing liquid was neutral, and the filter cake was mixed with acetone and 120 mL of n-hexane mixed solvent was used for recrystallization. The volume ratio of acetone to n-hexane in the mixed solvent used was 1:3 to obtain 15.1 g of 3-methylanthrone solid with a yield of 73.1% and a purity of 9...

Embodiment 3

[0053] (1) Synthesis of 3-methylanthrone

[0054] Add 2-methylanthraquinone (0.1mol, 22.2g), tin particles (0.2mol, 23.8g) and 200mL of acetic acid into a 500mL three-neck flask. The amount of acetic acid added is not specifically limited, and it can dissolve 2-methylanthraquinone That's it. 60mL of 37% (mass) concentrated hydrochloric acid was added under stirring at a temperature of 20-25°C, heated to 130°C, and stirred at a temperature of 130°C for 2h. After cooling to 25°C, pour the reaction solution into 100mL of water, and solids precipitated out. The reaction solution was left to stand and filtered to obtain a filter cake. The filter cake was washed with 100mL of water until the washing liquid was neutral, and the filter cake was mixed with acetone and 120 mL of n-hexane mixed solvent was used for recrystallization. The volume ratio of acetone to n-hexane in the mixed solvent used was 1:3 to obtain 15.1 g of 3-methylanthrone solid with a yield of 73.1% and a purity of ...

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Abstract

The invention discloses a method for synthetizing 3, 3'-dimethyl-9, 9'-dianthranide. The method includes the following steps of firstly, adding 2-tectoquinone, acetic acid, tin granules and 37% (mass) of concentrated hydrochloric acid into a reactor bottle, stirring to react for 1-3 hours at the temperature of 130 DEG C, cooling, pouring reaction liquid into water, filtering and recrystallizing to obtain 3-methyl anthrone solids; secondly, adding the obtained methyl anthrone solids, acetic acid, grained metal and 37% (mass) of concentrated hydrochloric acid into the reaction bottle, stirring to react for 1-3 hours at the temperature of 130 DEG C, cooling, filtering and recrystallizing to obtain 3, 3'-dimethyl-9, 9'-dianthranide, wherein the grained metal is zinc granules or tin granules, mole ratio of the 3-methyl anthrone to the metal is 1:3 to 1:10. The method is mainly used for preparing 3, 3'-dimethyl-9, 9'-dianthranide.

Description

technical field [0001] The invention relates to a synthesis method of 3,3'dimethyl-9,9'-bianthracene, which is mainly used in organic electroluminescent materials. Background technique [0002] Since the research group of C.W.Tang and S.A.VanSlyke of Eastman Kodak Company in the United States successfully made the first OLED device with good performance in 1987, organic electroluminescence display has entered a new stage of development with its outstanding advantages. In order to realize full-color display, high color purity and high efficiency red, green and blue primary color materials are necessary conditions. At present, the research progress of blue light materials is slower than that of green light and red light materials, because blue light materials require a wider energy gap, and it is more difficult to obtain blue light emission. Molecular design requires that the material has a certain degree of conjugated structure, but the dipole moment of the molecule should n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C15/28C07C1/207
Inventor 徐茂梁姜菡雨张倩张创军胡琳琳安忠维
Owner XIAN MODERN CHEM RES INST