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Process for producing 2-nitryl fluorenone

The technology of nitrofluorenone and fluorenone is applied in the field of aromatic organic compounds, can solve the problems of difficult separation and purification of reactants, difficult product purification, large environmental pollution and the like, and achieves high yield, low cost and little environmental pollution. Effect

Inactive Publication Date: 2008-08-20
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has used organic solvent acetic anhydride in the synthetic process, and environmental pollution is big, and productive rate is low, generates a large amount of by-product 4-nitrofluorenone, and product purification is difficult
[0007] Obviously, in the above-mentioned preparation method, there are problems such as low yield, high cost, difficulty in separation and purification of reactants, and environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Reagents: fluorenone, technical grade; concentrated nitric acid (65-68%), technical grade; concentrated sulfuric acid (96-98%), technical grade; ethanol, chemically pure.

[0016] Steps:

[0017] Add 9.00g (0.05mol) fluorenone and 15mL water into a 250mL four-necked round bottom flask equipped with a mechanical stirrer, reflux condenser, thermometer and constant pressure dropping funnel, start stirring, and heat until the temperature rises to 75°C Gradually add the mixed acid made of 10mL of concentrated nitric acid and 10mL of concentrated sulfuric acid dropwise, about 0.5h to complete the dropwise addition, control the system temperature at 85°C for 1.5h, add 150mL of water, cool to room temperature, suction filter, wash with water, dry, A yellow solid crude product was obtained, which was recrystallized from ethanol and dried to obtain 10.72 g of a pure product with a yield of 95.3% and a purity of 99.5%.

Embodiment 2

[0019] Reagent: with embodiment 1.

[0020] Steps:

[0021] Add 9.00g (0.05mol) fluorenone and 15mL water into a 250mL four-necked round bottom flask equipped with a mechanical stirrer, reflux condenser, thermometer and constant pressure dropping funnel, start stirring, and heat until the temperature rises to 75°C Gradually add the mixed acid made of 10mL concentrated nitric acid and 10mL concentrated sulfuric acid dropwise, about 0.5h to complete the dropwise addition, control the system temperature at 120°C for 1.5h, add 150mL water, cool to room temperature, suction filter, wash with water, dry, A yellow solid crude product was obtained, which was recrystallized from ethanol and dried to obtain 10.26 g of pure product with a yield of 91.2% and a purity of 99.0%.

[0022] Recycling of ethanol: The ethanol used for recrystallization can be reused after distillation.

[0023] Physical constants and spectral data of the product: Appearance: yellow solid; melting point: 222-22...

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Abstract

A method for preparing 2-nitrofluorenone from fluorenone comprises the following steps, a certain amount of fluorenone and water are added into a reactor, after the temperature increasing to 75 DEG C, the mixed acid of concentrated nitric acid and concentrated sulfuric acid is dripped, the temperature of the system is controlled between 80 to 120 DEG C with the reaction time of 0.5 to 3 hours, cooled, pumped by air, filtered, washed by water, and dried, yellow solid raw product which is then recrystallized is obtained and pure product is obtained after being dried; the yield of the product through the method is 91.0 to 96.0 percent, the purity is more than 99 percent; the preparation method has the advantages of easy operation, easy separation and purification of products, high yield, low cost, and little environment pollution.

Description

technical field [0001] The invention relates to an aromatic organic compound, in particular to a method for preparing 2-nitrofluorenone from fluorenone. Background technique [0002] As an important fine chemical intermediate, 2-nitrofluorenone is widely used in the preparation of pesticides, dyes, medicines and functional polymer materials. At present, the preparation method of relevant report 2-nitrofluorenone at home and abroad mainly contains the following aspects: [0003] (1) Using 2-methyl-4-nitrobiphenyl as a raw material, 2-nitrofluorenone (Synthesis, 1989, 3: 184-188) was prepared by bromination, oxidation, acylation and other reactions; -Iodine-N-(4'-nitrobiphenyl-2-methyleneamino)aniline is used as raw material, and 2-nitrofluorenone (J.Am.Chem.Soc., 2007, 129(16):5288-5295). The preparation method is complex in operation, high in cost, and difficult to realize industrialization. [0004] (2) Using fluorene as raw material, carry out nitration reaction in org...

Claims

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Application Information

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IPC IPC(8): C07C205/45C07C201/08
Inventor 张昭张鑫秦利平韩俊斌
Owner SHANXI UNIV