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Preparation method of 1,2-dichloro-4-nitrobenzene

A technology of nitrobenzene and p-nitrochlorobenzene, which is applied in 1 field, can solve the problems of environmental pollution, cumbersome steps, and low yield, and achieve the effects of increased product yield, simple synthesis process, and mild reaction conditions

Inactive Publication Date: 2020-04-07
陶丽琼
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  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the existing 1,2-dichloro-4-nitrobenzene preparation method of environmental pollution, complicated steps, low yield problems, to provide a simple process, high yield, reaction Preparation method of 1,2-dichloro-4-nitrobenzene under mild conditions

Method used

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Embodiment Construction

[0008] A preparation method of 1,2-dichloro-4-nitrobenzene of the present invention, in particular: put p-nitrochlorobenzene into a sulfuric acid solution with a mass fraction of 65%, stir and dissolve, heat up to 55°C, and then Add potassium chlorate, stir and keep warm for 7 hours. After the reaction is complete, cool down with ice water, use carbon tetrachloride solution to extract the reaction solution, and use 6% sulfurous acid aqueous solution and 12% hydrogen for the organic phase after liquid separation. Wash with sodium oxide aqueous solution and water, dry again, evaporate the organic solution to dryness, recrystallize to obtain yellow needle crystals, which is the product 1,2-dichloro-4-nitrobenzene.

[0009] In this embodiment, the mass ratio of p-nitrochlorobenzene and potassium chloride acid is 1:1.

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Abstract

The invention discloses a preparation method of 1,2-dichloro-4-nitrobenzene. The preparation method comprises the following steps: adding p-nitrochlorobenzene into a sulfuric acid solution with a massfraction of 65%, carrying out stirring for dissolving of the p-nitrochlorobenzene, conducting heating to 55 DEG C, then adding potassium chlorate, carrying out a stirring and heat-preserved reactionfor 8 h, performing cooling with ice water after the reaction is completed, extracting a reaction solution with a carbon tetrachloride solution, conducting liquid separation, subjecting an organic phase to washing by an aqueous sulphurous acid solution with a mass fraction of 6%, an aqueous sodium hydroxide solution with a mass fraction of 12% and water in sequence, carrying out drying, evaporating an organic solution to dryness, and performing recrystallizing to obtain a yellow acicular crystal, namely the product 1,2-dichloro-4-nitrobenzene. The preparation method is simple in synthesis process, improved in product yield and mild in reaction conditions, and has practical application and promotion values.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, in particular to a preparation method of 1,2-dichloro-4-nitrobenzene. Background technique [0002] 1,2-Dichloro-4-nitrobenzene is mainly used in the synthesis of fluoroaniline, an important fluorine-containing pharmaceutical intermediate. There are two main ways to synthesize 1,2-dichloro-4-nitrobenzene: (1) Direct chlorination of p-nitrochlorobenzene: Chlorine is a commonly used chlorination agent in this type of reaction, but due to the The existence of the electron-withdrawing group-NO2 requires relatively harsh reaction conditions, which increases the number of side reactions, and the operation is relatively cumbersome, and the product yield is low; (2) Direct nitration of ortho-dichlorobenzene: use nitric acid and sulfuric acid to carry out dichlorobenzene Nitrification, yellow needle-like crystals are obtained after recrystallization with ethanol or carbon tetrachloride, but th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/12C07C201/12
CPCC07C201/12C07C205/12
Inventor 吴凯黄焕军严学文陶丽琼
Owner 陶丽琼
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