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Method for preparing substituted dibenzyl ether

A technology of dibenzyl ether and benzyl halide, which is applied in the field of preparation of substituted dibenzyl ethers, can solve the problems of lack of competitiveness, consume a large amount of alkali, and not involve the preparation method of substituted dibenzyl ethers, and reduce resource consumption , The effect of reducing waste discharge

Inactive Publication Date: 2006-09-20
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Experimental program
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Effect test

Embodiment 1

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

[0030] Take 2.53g of chlorobenzyl chloride, 0.10g of KI, and 18mL of water into the Erlenmeyer flask, quickly heat to 115℃, start refluxing, stir vigorously, reflux for 48 hours, the reaction pressure is 5 MPa, TLC detection (ethanol-n-hexane, 1:5), the composition no longer changes. The temperature was lowered to about 60°C, 20mL of toluene was added for extraction, the temperature was approaching room temperature, and the liquid was separated. The aqueous phase is extracted with ethyl acetate (10 mL×2) to recover hydrogen halide; the organic phases are combined, dried over anhydrous sodium sulfate, and evaporated to dryness (if a small amount of water remains, 10-20 mL of toluene can be added and evaporated to dryness). After passing through a silica gel column (the method and parameters of passing the silica gel column are known to those of ordinary skill in the art), 1.25 g of a colorless oily p...

Embodiment 2

[0031] Example 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 colorless oily product was obtained, and 0.78 g of 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 the raw 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 invention relates to a method for preparing substituted dibenzyl ethers, wherein a substituted benzyl halide is used to react with water, particularly a method for generating substituted dibenzyl ethers catalyzed by a metal halide. 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 base fragrances in fine chemicals. The 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 a light soil aroma or a mushroom aroma with a rose-like base. It can be added to cosmetics, food and beverages, etc., and is safe and reliable. [0003] Various preparation methods of dibenzyl ether have been widely seen in the open literature....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/01C07C43/164C07C43/174
Inventor 李振江韦萍万红贵任星华石玉瑚欧阳平凯
Owner NANJING TECH UNIV
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