The preparation method of 4,4'-dimethyl dibenzyl ether

A technology of dimethyl dibenzyl ether and p-methyl benzyl chloride, which is applied in the field of preparation of 4,4'-dimethyl dibenzyl ether, can solve the problems of low efficiency and long reaction time, and achieve simplified reactions Process, short reaction time, high stability effect

Active Publication Date: 2016-08-24
WUHAN YOUJI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But in method (2), raw material alcohol is obtained by the hydrolysis of raw material halogenated hydrocarbon, and reaction time is longer, and efficient is low

Method used

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  • The preparation method of 4,4'-dimethyl dibenzyl ether

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Embodiment 1

[0023] A kind of preparation method of 4,4'-dimethyl dibenzyl ether, it comprises the following steps successively:

[0024] 1) In a 1000mL glass reaction bottle, first add 281g of p-methylbenzyl chloride (purity: 99.0%, 2.0mol), then add 480g (3.0mol) of NaOH solution with a mass percentage concentration of 25%, and add 5.6 g tetrabutylammonium bromide (purity is 99.0%), heated up to 110°C under stirring, and refluxed for 6 hours;

[0025] 2) The reaction material was cooled to room temperature under stirring, white crystals were precipitated, and the obtained white solid was dried in the air to obtain 246.5 g of crude product; the purity of 4,4'-dimethyldibenzyl ether in the crude product was 90.40% (GC) , the yield is 98.6%;

[0026] 3) Take 50.0 g of the crude product of 4,4'-dimethyldibenzyl ether and place it in a 500 ml four-neck flask, add 25 g of 95.0% (purity, GC) ethanol, heat to reflux, and stop heating after all the solids are dissolved , continue to stir and co...

Embodiment 2

[0029] A kind of preparation method of 4,4'-dimethyl dibenzyl ether, it comprises the following steps successively:

[0030] 1) In a 1000mL glass reaction bottle, first add 281g of p-methylbenzyl chloride (purity: 99.0%, 2.0mol), then add 480g (3.0mol) of NaOH solution with a mass percentage concentration of 25%, and add 5.2 g triethylamine heated to 110° C. under stirring, and refluxed for 6 hours;

[0031] 2) The reaction material was cooled to room temperature under stirring, white crystals were precipitated, and the obtained white solid was air-dried to obtain 215.2 g of crude product; the purity of 4,4'-dimethyldibenzyl ether was 96.39% (GC), The yield is 91.8%;

[0032] 3) Take 50.0 g of the crude product of 4,4'-dimethyldibenzyl ether and place it in a 500 ml four-neck flask, add 25 g of 95.0% (purity, GC) ethanol, heat to reflux, and stop heating after all the solids are dissolved , continue to stir and cool to room temperature, a white solid is precipitated, suction...

Embodiment 3

[0035] A kind of preparation method of 4,4'-dimethyl dibenzyl ether, it comprises the following steps successively:

[0036] 1) In a 500mL glass reaction bottle, first add 70.3g of p-methylbenzyl chloride (purity: 99.0%, 0.5mol), then add 150g (0.75mol) of NaOH solution with a mass percentage concentration of 20%, and add 1.1g of tetrabutylammonium bromide, heated to 108°C under stirring, and refluxed for 6 hours;

[0037] 2) The reaction material was cooled to room temperature under stirring, white crystals were precipitated, and the obtained white solid was air-dried to obtain 63 g of crude product; the purity of 4,4'-dimethyldibenzyl ether was 93.35% (GC), and the obtained The rate is 104%.

[0038] 3) Take 50.0 g of the crude product of 4,4'-dimethyldibenzyl ether and place it in a 500 ml four-neck flask, add 25 g of 95.0% (purity, GC) ethanol, heat to reflux, and stop heating after all the solids are dissolved , continue to stir and cool to room temperature, a white sol...

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Abstract

The invention discloses a method for preparing 4, 4'-dimethyl dibenzyl ether. The method comprises the following steps: 1) adding p-methyl benzyl chloride, an alkali solution and a phase transfer catalyst in a reaction vessel, and full reacting at 106-122 DEG C; 2) cooling and crystallizing reaction liquid, conducting pumping filtration and air drying to obtain a 4,4'-dimethyl dibenzyl ether crude product; and 3) recrystallizing the 4, 4'-dimethyl dibenzyl ether crude product to obtain the 4,4'-dimethyl dibenzyl ether finished product. The preparation method has simple process, high efficiency, and low production cost, and is easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of manufacturers of organic chemical products, and specifically refers to a preparation method of 4,4'-dimethyl dibenzyl ether. Background technique [0002] 4,4'-Dimethyldibenzyl ether is the raw material for the preparation of p-tolualdehyde, which is an important fine chemical and organic chemical intermediate, mainly used in perfumes, triphenylmethane dyes etc. synthesis. [0003] There are few reports on the synthesis of 4,4'-dimethyldibenzyl ether, but there are many reports on the synthesis of aromatic ethers such as anisole, which is a similar compound. The common ones are as follows: (1) dehydration reaction between alcohol and phenol molecules (comprising normal pressure method and high pressure method), as the date of application is July 8, 1998, the publication number is CN1267277A, and the name is called "benzyl type alcohol The etherification method and the product obtained by the method and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/164C07C41/01
CPCC07C41/01C07C43/164
Inventor 孙波陈乐黄正望杨勇王瑞君舒振操毛利民
Owner WUHAN YOUJI IND
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