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: 2015-07-08
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 fluorene oxide, 170ml of ethylene glycol dimethyl ether, 11.5g (0.5mol) of sodium metal into a 500ml three-necked flask, N 2 Under protection, react at 80°C for 6h, cool the reaction mixture to below 70°C, add 10ml ethanol, stir for 30 minutes, distill to recover the solvent, then add 100ml of water to the residue, cool to room temperature, filter and recover unreacted raw materials, for water phase use Adjust the pH to less than 3 with concentrated hydrochloric acid, and a brown oil precipitated, extracted with ethyl acetate, dried over anhydrous sodium sulfate, removed the solvent under reduced pressure, recrystallized with petroleum ether to obtain 34.9g of o-phenylphenol, the content was greater than 99%, the yield 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 synthetic method for preparing o-phenylphenol by ring opening of fluorene oxide. Background technique [0002] At present, the production of o-phenylphenol at home and abroad mainly adopts cyclohexanone condensation dehydrogenation method. 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 shortcomings. The 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 a supported precious metal as a catalyst, and the cost of the catalyst is relatively high, and after 100 ...

Claims

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Application Information

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