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Method for preparing 2-bromofluorenone by catalyzing oxidizing of molecular oxygen in water phase

A technology for bromofluorenone in aqueous phase, applied in the field of 2-bromofluorenone synthesis, can solve problems such as toxicity, environmental pollution, danger, etc., and achieve the effects of less waste, high catalytic activity, and strong industrial application prospects

Active Publication Date: 2018-07-13
XINXIANG RUNYU NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As an important part of traditional chemical production, organic solvents have certain toxicity and danger, and are the main source of waste in chemical synthesis, which will cause serious environmental pollution

Method used

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  • Method for preparing 2-bromofluorenone by catalyzing oxidizing of molecular oxygen in water phase
  • Method for preparing 2-bromofluorenone by catalyzing oxidizing of molecular oxygen in water phase
  • Method for preparing 2-bromofluorenone by catalyzing oxidizing of molecular oxygen in water phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Catalytic oxidation of 2-bromofluorene to synthesize 2-bromofluorenone.

[0022] In a 50L glass reactor equipped with a reflux condenser and mechanical stirring, add 5Kg 2-bromofluorene, 0.5g Salen manganese catalyst, 0.5g Salen cobalt catalyst and 30L water, heat to 80°C while stirring, and bubble in air to react After 16 hours, the reaction was stopped, cooled, filtered, and the filter cake was dried to obtain 5.2Kg of a yellow solid. 1 H-NMR and 13 The structure was determined to be 2-bromofluorenone by C-NMR, and the yield was 99%. The purity of the product analyzed by liquid chromatography was 99.8%. The aqueous phase obtained by filtration was retained and continued to be used in the next batch.

Embodiment 2

[0023] Example 2: Synthesis of 2-bromofluorenone by catalytic oxidation of 2-bromofluorene in the aqueous phase recovered by filtration.

[0024] In a 50L glass reactor equipped with a reflux condenser and mechanical stirring, add 5Kg 2-bromofluorene, 0.5g Salen manganese catalyst, 0.5g Salen cobalt catalyst and the water phase recovered by filtration in Example 1, and heat to 80°C under stirring , feed air bubbles, stop the reaction after 16 hours of reaction, cool, filter, and dry the filter cake to obtain 5.2Kg of yellow solid. 1 H-NMR and 13 The structure was determined to be 2-bromofluorenone by C-NMR, and the yield was 99%. The purity of the product analyzed by liquid chromatography was 99.6%. The aqueous phase mother liquor obtained by filtration is retained and used in the next batch.

Embodiment 3

[0025] Example 3: Catalytic oxidation of 2-bromofluorene to synthesize 2-bromofluorenone.

[0026] In a 50L glass reactor equipped with a reflux condenser and mechanical stirring, add 5Kg 2-bromofluorene, 1g Salen cobalt catalyst and 30L water, heat to 100°C while stirring, and bubble in air, and stop the reaction after 24 hours of reaction , cooled, filtered and dried to obtain 5.0Kg of yellow solid, the product was 1 H-NMR and 13 C-NMR confirmed the structure as 2-bromofluorenone, and the yield was 98.5%.

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Abstract

The invention provides a method for preparing 2-bromofluorenone by catalyzing oxidizing of molecular oxygen in a water phase. The method is characterized in that a transition metal Salen ligand is used as a catalyst; under the condition of air bubbles, 2-bromofluorene is oxidized to generate the 2-bromofluorenone in the water phase, the reaction temperature is 60 to 100 DEG C, and the reaction time is 8 to 24h. The method has the advantages that the reaction is performed in the water phase, the organic solvent as the reaction medium is not needed, and the environment-friendly effect is betterin comparison with the traditional oxidizing method; the transition metal Salen catalyst has higher catalytic activity in the water phase medium; the water phase medium can be utilized for multiple times, the amount of wastes is fewer, and the industrial application prospect is stronger.

Description

technical field [0001] The invention belongs to the technical field of 2-bromofluorenone synthesis, and in particular relates to a method for preparing 2-bromofluorenone by catalyzing molecular oxygen oxidation in an aqueous phase. Background technique [0002] The performance research of electroluminescent materials has attracted much attention in recent years, among which fluorene derivatives have aroused extensive research interest of material scientists. Due to the advantages of easy modification, good solubility and film-forming properties, excellent optical stability and thermal stability, and high luminous efficiency, fluorene derivatives have great commercial value in the research field of electroluminescent materials. 2-Bromofluorenone is one of the very important intermediates in fluorene-based electroluminescent materials, and its synthesis process and product quality directly affect various properties of fluorene-based electroluminescent materials. [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/36C07C49/697
CPCC07C45/36C07C49/697
Inventor 耿巍芝
Owner XINXIANG RUNYU NEW MATERIAL TECH CO LTD
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