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Method for preparing 9-fluorenone via four-phase transfer catalysis

A technology of phase transfer catalysis and fluorenone, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of large solvent loss, difficult phase transfer catalyst effect of quaternary ammonium salts, and high reaction temperature. achieve the effect of improving utilization efficiency

Active Publication Date: 2013-12-11
BAOSHUN TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is that without adding water, the quaternary ammonium salt is difficult to play the role of phase transfer catalyst, the reaction temperature is high, and the solvent loss is large; the document does not disclose the type of quaternary ammonium salt and other issues

Method used

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  • Method for preparing 9-fluorenone via four-phase transfer catalysis
  • Method for preparing 9-fluorenone via four-phase transfer catalysis
  • Method for preparing 9-fluorenone via four-phase transfer catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Take 40g of industrial fluorene and place it in a 250mL four-necked flask equipped with mechanical stirring, reflux condenser, and two inlet pipes, add 45mL of xylene, 0.72g of tetrabutylammonium chloride and 9mL of 40wt% NaOH solution, and place in a water bath at 40°C Heating at medium temperature, controlling the stirring rate to 300r / min, feeding 200*2mL / min air, and connecting the outlet of the reflux condenser tube to the inlet of the tail gas absorption tube equipped with α-methylnaphthalene. At the beginning of the reaction, fluorene was suspended. The reaction process was monitored by thin chromatography, and the raw material fluorene spots disappeared after 6 hours of reaction, and the reaction was continued for 0.5 hours to stop the reaction. The reaction liquid was transferred to a 500mL beaker while it was hot, and pale yellow crystals were precipitated immediately. After no more crystals were precipitated, vacuum filtration was performed to obtain crystal ...

Embodiment 2

[0058] Except that raw material fluorene is increased to 80g, and tetrabutylammonium chloride is increased to 1.7g, other is the same as embodiment 1. After 8 hours of reaction, TLC showed that the raw material fluorene spots completely disappeared, and the reaction was continued for 0.6 hours to stop the reaction.

[0059] 64.08 g of crystal i was obtained, and the content of 9-fluorenone was >99.5% according to chromatographic analysis;

[0060] Crystal II weighed 15.1 g, and the 9-fluorenone content was 97% according to chromatographic analysis.

Embodiment 3

[0062] Except that raw material fluorene is increased to 60g, other is the same as embodiment 1. After 7 hours of reaction, thin-layer chromatography showed that the raw material fluorene spots completely disappeared, and the reaction was continued for 0.5 hours to stop the reaction.

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Abstract

The invention discloses a method for preparing 9-fluorenone via four-phase transfer catalysis. At a lower temperature, alkali is taken as a catalyst, quaternary ammonium salt serves as a phase transfer agent, fluorene can be excessive and reacts with oxygen-containing gas in xylene in states of dissolution and suspension, and high-purity 9-fluorenone is directly obtained, a right reaction condition is selected, and the transformation rate of the fluorene can reach 100 percent. According to the invention, the recovered alkali and the dissolvent do not need to be treated complexly and particularly, reuse can be realized, and industrialization is facilitated; in addition, mixed xylene and water are taken as the dissolvent, the oxidation of the fluorene as the reaction condition of the 9-fluorenone, the selection of the catalyst alkali and phase transfer agent, and the reuse of the dissolvent and the alkali are researched, as a result, the conditions of high transmission rate of fluorene and high selective transmission of the 9-fluorenone are obtained, and a more complete compounding process is disclosed.

Description

technical field [0001] The invention relates to a method for preparing 9-fluorenone by four-phase phase transfer catalysis, which belongs to the field of organic synthesis. Background technique [0002] Fluorene is one of the important components of coal tar, accounting for 1% to 2% of the total amount of coal tar. The price of fluorene itself is relatively cheap. With the intensification of market competition among enterprises, businesses have higher and higher requirements for the purity of fluorene. The crude fluorene separated from tar can no longer meet the requirements. If it continues to be deeply purified, the production cost will be too high. High, will affect the development of enterprises. Therefore, it is imperative to develop high value-added fluorene downstream products using fluorene with a content of ≥95% from coal tar as the starting material. 9-fluorenone is a good deep-processing product of fluorene, and it is an important chemical raw material. Many flu...

Claims

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Application Information

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IPC IPC(8): C07C49/675C07C45/36
Inventor 高占先于丽梅闫俊李汇丰何永超
Owner BAOSHUN TECH CO LTD
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