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Process for synthesizing1,3,5-triphenyl benzene

A triphenylbenzene, a new synthesis technology, applied in 1 field, can solve the problems of waste of energy and high-purity nitrogen, long reaction time, reduced yield and the like, and achieve the effects of easy recovery, easy operation, and reduced production costs

Inactive Publication Date: 2006-09-27
YANGZHOU UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The strong acid used in the common strong acid catalyzed synthesis of 1,3,5-triphenylbenzene is an acid with good dehydration effect such as concentrated sulfuric acid, and it needs to be heated for more than 10 hours with an acid with an equal molar amount to complete the reaction. There is a strong carbonization effect under heating, and a large part of the raw materials are converted into black carbon, which not only reduces the yield of the reaction but also obtains a large amount of black substances that pollute the environment
[0005] Silicon tetrachloride and aluminum trichloride can also be catalyzed to synthesize this type of reaction, but both silicon tetrachloride and aluminum trichloride have strong water absorption, and this type of reaction needs to be carried out under nitrogen protection, which makes the operation The process requires cumbersome equipment such as glove boxes and anhydrous and oxygen-free nitrogen protection devices. At the same time, the dehydration of such substances is worse than that of concentrated sulfuric acid, so it is necessary to add equivalent catalysts and the reaction time is relatively long. In case of reaction for more than 24 hours, a lot of energy and high-purity nitrogen will be wasted

Method used

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  • Process for synthesizing1,3,5-triphenyl benzene

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Embodiment Construction

[0018] Reaction formula of the present invention is:

[0019]

[0020] where R=(a)C 6 h 5 ; (b) 4-MeC 6 h 4 ; (c) 4-MeOC 6 h 4 ; (d) 4-ClC 6 h 4 ; (e) 4-BrC 6 h 4 ; (f)-Me; (g)4-NO 2 C 6 h 4

[0021] Specific steps:

[0022] Dissolve 1.2g of acetophenone in 10ml of dry anhydrous n-amyl alcohol, to prevent the water from destroying the tin tetrachloride added later and make the catalyst lose its effect, slowly drop in 5% mol of the catalyst tin tetrachloride under stirring, and then Add 5% mol of catalyst p-toluenesulfonic acid to form a composite catalyst. The amount is enough to ensure the normal progress of the reaction. React for 5 hours at a temperature of 110°C. After the reaction is completed, pour the reactant into 20ml of absolute ethanol , because the solubility of the product triphenylbenzene compound in ethanol is relatively small, so the product will be separated out in a large amount, then the ethanol solution is put into the refrigerator and cool...

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Abstract

The invention discloses a 1, 3, 5-triphenyl benzene synthesizing method, which comprises the following steps: dissolving acetophenone in n-amyl alcohol; mixing and adding in accelerant tin tetrachloride; putting in accelerant p-toluenesulfonic acid; reacting at 110deg.c for hours; pouring out reactant in absolute ethyl alcohol; mixing; filtering; using carrene-alcohol for recrystallization; getting 1,3,5-diphenylbenzene benzene. The invention solves the problem of the carbonization of corrosive acid catalystsing and synthesizing 1, 3, 5-triphenyl benzene, which reduces the reaction yield and environmental contamination.

Description

technical field [0001] The present invention relates to 1,3,5-triphenylbenzene, in particular to a synthesis method of 1,3,5-triphenylbenzene. Background technique [0002] 1,3,5-Triphenylbenzene is a class of aromatic compounds with a special structure. It is an important basic functional module for the construction of dendrimers, organic conductive polymers and polarized nonlinear optical materials. It is also a class of promising electroluminescent organic molecular materials. [0003] Prior to the present invention, the synthesis method of 1,3,5-triphenylbenzene included the use of rare earth chlorides, strong acids, silicon tetrachloride and aluminum trichloride to catalyze the synthesis of acetophenone trimolecular condensation. However, most of these reactions have defects such as cumbersome operation, harsh reaction conditions, or long reaction time. The specific performance is as follows: [0004] The strong acid used in the common strong acid catalyzed synthesis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/42C07C15/14
Inventor 景崤壁徐峰朱启华杨进
Owner YANGZHOU UNIV
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