Method for preparing o-phenyl phenol by ring opening of dibenzofuran

A technology of o-phenylphenol and oxyfluorene, which is applied in the synthesis field of oxyfluorene ring-opening to prepare o-phenylphenol, can solve the problems of non-industrialization, industrialization significance, increased production cost, expensive metal lithium, etc. Prospect, low cost, good effect

Active Publication Date: 2013-09-25
LIAONING PETROCCHEM VOCATIONAL & TECH COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lithium metal is expensive, and from the perspective of production cost, it has no industrialization and industrialization significance
[0007] The above synthesis process generally requires high temperature and high pressure conditions, requires special reactors, and uses noble metal catalysts or expensive alkali metals as raw materials, all of which increase production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 42.8g (0.25mol, 99%) of dioxyfluorene, 170ml of ethylene glycol dimethyl ether, 11.5g (0.5mol) of sodium metal, and N 2 Under protection, react at 80°C for 6 hours, cool the reaction mixture to below 70°C, add 10ml of ethanol, stir for 30 minutes, distill and recover the solvent, then add 100ml of water to the residue, cool to room temperature, filter and recover unreacted raw materials, and use for the water phase Adjust the pH to less than 3 with concentrated hydrochloric acid, and a brown oil is precipitated, extracted with ethyl acetate, dried over anhydrous sodium sulfate, removed the solvent under reduced pressure, and recrystallized with petroleum ether to obtain 34.9 g of o-phenylphenol, the content is greater than 99%, and the yield is 82.0%.

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PUM

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Abstract

The invention relates to a synthetic method for preparing o-phenyl phenol by ring opening of dibenzofuran. The synthetic method comprises the following steps: using dibenzofuran as a raw material, using glycol dimethyl ether or diethylene glycol dimethyl ether as a solvent, adding metallic sodium, reacting under the protection of nitrogen, adjusting pH to less than 3 by adding aqueous phase concentrated hydrochloric acid, precipitating a brown oily matter, extracting by the use of ethyl acetate, drying by the use of anhydrous sodium sulfate, carrying out pressure reduction to remove the solvent, and recrystallizing by the use of petroleum ether so as to obtain o-phenyl phenol. The method provided by the invention has advantages of high yield, relatively low cost and good effect, and has a wide application prospect.

Description

technical field [0001] The invention belongs to the field of organic chemical industry, and more specifically relates to a synthesis method for preparing o-phenylphenol by ring opening of oxyfluorene. Background technique [0002] At present, the production of o-phenylphenol at home and abroad mainly adopts the condensation dehydrogenation method of cyclohexanone. Chinese Patent Publication No. CN1371897A discloses a method for synthesizing o-phenylphenol from cyclohexanone. Cyclohexanone is condensed under strong acid catalysis, and the resulting dimer is catalytically dehydrogenated in a tubular reactor to obtain o-phenylphenol. However, this method has obvious disadvantages. Dehydrogenation is generally carried out at a high temperature of 290-350°C, the reaction conditions are harsh, the equipment investment is high, and the energy consumption is large. The reaction uses supported noble metals as catalysts, and the cost of the catalysts is relatively high, and after 100...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/06C07C37/055
Inventor 杨连成
Owner LIAONING PETROCCHEM VOCATIONAL & TECH COLLEGE
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