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Method for preparing substituted dibenzyl ether

A technology of dibenzyl ether and benzyl halide, applied in the field of preparation of substituted dibenzyl ether, can solve the problems of lack of competitiveness, consumption of a large amount of alkali, and no preparation method of substituted dibenzyl ether, etc., and reduce resource consumption. , the effect of reducing waste emissions

Inactive Publication Date: 2005-12-21
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process produces a small amount of dibenzyl ether as a by-product, and a feature disclosed in the above-mentioned patent is that the by-product dibenzyl ether is rarely produced under the condition of lower conversion rate, making other processes economically uncompetitive
And, above-mentioned technological method all does not relate to the preparation method of relevant substituted dibenzyl ether, and their common limitation is to consume a large amount of alkali, or need special reagent and facility

Method used

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  • Method for preparing substituted dibenzyl ether
  • Method for preparing substituted dibenzyl ether

Examples

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Effect test

Embodiment 1

[0029] Embodiment 1: Preparation of dibenzyl ether by hydrolysis of benzyl chloride

[0030] Take 2.53g of chlorobenzyl chloride, KI0.10g, and 18mL of water into the conical flask, rapidly raise the temperature to 115°C, start to reflux, vigorously stir, and reflux for 48 hours, the reaction pressure is 5 MPa, TLC detection (ethanol-n-hexane, 1:5), the composition does not change. Cool down to about 60°C, add 20mL of toluene for extraction, the temperature will be close to room temperature, and separate the liquids. The aqueous phase was extracted with ethyl acetate (10mL×2) to recover hydrogen halide; the organic phases were combined, dried over anhydrous sodium sulfate, and fully evaporated to dryness (if a small amount of water remained, add 10-20mL of toluene and evaporate to dryness). After passing through a silica gel column (the method and parameters of passing through a silica gel column are well known to those skilled in the art), 1.25 g of a colorless oily product w...

Embodiment 2

[0031] Embodiment 2: Preparation of dibenzyl ether by hydrolysis of benzyl bromide

[0032] The method of Example 1. But the raw material benzyl bromide (3.42g) was reacted for 24 hours. 1.33 g of a colorless oily product was obtained, and 0.78 g of the raw material was recovered.

Embodiment 3

[0033] Example 3: Preparation of 4,4'-dichlorobenzyl ether by hydrolysis of 4-chlorobenzyl chloride

[0034] The method of Example 1. But starting material 4-chlorobenzyl chloride (3.22g), KI (0.17g), reacted for 24 hours. 1.70 g of colorless needle crystal product was obtained, and 0.91 g of raw material was recovered.

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Abstract

This invention has disclosed a kind of producing method for substituted dibenzyl ether. This method adopts substituted benzyl halogen react with water to produce substituted dibenzyl ether directly by the catalyst of metal halide. It does not use alkali substance, after separate and concentrate, procreant HX can be regenerated. This method is simple and environmental protection, costs little.

Description

technical field [0001] The present invention relates to a preparation method of substituted dibenzyl ether, wherein the reaction of substituted benzyl halide and water, especially the method of metal halide catalysis, is used to generate substituted dibenzyl ether. Background technique [0002] Dibenzyl ether and its derivatives are used as plasticizers for nitrocellulose and functional coatings, as additives in rubber and textile industries, and as solvents and primers for fragrances in fine chemicals. Dibenzyl ether derivatives with functional groups can be used in organic synthesis to prepare a variety of biologically active compounds. These are well known to those skilled in the art. For example, dibenzyl ether itself has a special aroma such as light earthy aroma or mushroom aroma with a rose-like base aroma, which can be added to cosmetics, food and beverages, etc., which is safe and reliable. [0003] The preparation of various dibenzyl ethers is widely described in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/164
Inventor 李振江韦萍万红贵任星华石玉瑚欧阳平凯
Owner NANJING UNIV OF TECH
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