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Method for synthesizing diphenoxyl methane

A technology of diphenoxymethane and dibromomethane, applied in the field of synthesizing diphenoxymethane under low temperature and normal pressure, can solve the problems of complex separation of products, low yield, long reaction time, etc., and achieve high added value, The effect of high purity and easy separation

Inactive Publication Date: 2011-04-06
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method introduces dimethyl sulfoxide as a solvent, which makes the separation of the product complicated, and dichloromethane and diiodomethane are used as raw materials, the reaction time is longer and the yield is low

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0013] The first step: 30.8g potassium hydroxide is added in the phenol of 47g fusion under vigorous stirring condition and stirs ten minutes;

[0014] Step 2: Add 42.5g of dibromomethane dropwise, heat and stir at 80°C for 2h;

[0015] The third step: the product is extracted with 60 ml of diethyl ether for several times, and the extract is mixed, distilled to remove the diethyl ether, and the remaining oily liquid is detected by GC and GC-MS to obtain diphenoxymethane.

Embodiment 2

[0017] The first step: 30.8g potassium hydroxide is added in the phenol of 47g fusion under vigorous stirring condition and stirs ten minutes;

[0018] Step 2: Add 42.5g of dibromomethane dropwise, heat and stir at 80°C for 3h;

[0019] The third step: the product is extracted with 60 ml of diethyl ether for several times, and the extract is mixed, distilled to remove the diethyl ether, and the remaining oily liquid is detected by GC and GC-MS to obtain diphenoxymethane.

Embodiment 3

[0021] The first step: 38g potassium hydroxide is added in the phenol of 47g melting under the vigorous stirring condition and stirs ten minutes;

[0022] Step 2: Add 42.5g of dibromomethane dropwise, heat and stir at 90°C for 2h;

[0023] The third step: the product is extracted with 60 ml of diethyl ether for several times, and the extract is mixed, distilled to remove the diethyl ether, and the remaining oily liquid is detected by GC and GC-MS to obtain diphenoxymethane.

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Abstract

The invention discloses a method for synthesizing diphenoxyl methane, comprising the following steps of: adding and strongly stirring potassium hydroxide to fused phenol, then slowly dropwise adding dibromomethane after stirring for ten minutes, stirring and making the mixture react for 2-5 h at 80-100 DEG C, extracting a reactant by using diethyl ether, and distilling to obtain a residual oily liquid which is the diphenoxyl methane. The method for synthesizing diphenoxyl methane is carried out at low temperature and normal pressure and has simple and easy operation and 100% of selection, andthe synthesized diphenoxyl methane has high purity and stable performance; and the invention provides a new approach for converting the diphenoxyl methane.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a method for synthesizing diphenoxymethane at low temperature and normal pressure. Background technique [0002] Diphenoxymethane, a kind of acetal compound, is a light yellow oily liquid at room temperature, with a boiling point of 292~293°C, and is miscible with most organic solvents such as alcohol, ether, and acetone. Acetal compounds are important intermediates in organic synthesis and important chemical raw materials, and can be used as oil additives without environmental problems; under suitable catalyst conditions, they can be directly oxidized to synthesize carbonates with molecular oxygen. [0003] The traditional method of synthesizing diphenoxymethane is to use phenol and diiodomethane or dichloromethane as raw materials, use dimethyl sulfoxide as a solvent, and add a phase transfer catalyst under the alkaline condition of sodium hydroxide to obtain diphenoxymethane. me...

Claims

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Application Information

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IPC IPC(8): C07C43/303C07C41/52
Inventor 单永奎申欢欢张恒强丁永杰孙卓东
Owner EAST CHINA NORMAL UNIV
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