Preparation method of 2-bromo-5-fluoro-4-nitroaniline

Abstract

The invention relates to the field of chemistry, in particular to a preparation method of 2-bromo-5-fluoro-4-nitroaniline. The method comprises the following steps: A, adding 1.3 parts of iron powder and 0.1 part of ammonium chloride into a reaction system, refluxing and adding 1 part of raw materials, adjusting the pH after the reaction is finished until the pH value reaches 9, and evaporating the water to obtain a product for later use; step B, adding 0.6 part of acetic anhydride with the concentration of 99% into 1 part of the product in the step A, heating to 80 DEG C, keeping the temperature for 1 hour, and reacting to obtain a product for later use; step C, adding 6.5 parts of 98% sulfuric acid into 1 part of the product in the step B, dropwise adding 0.4 part of nitric acid, reacting at 20-30 DEG C for 1 hour, and performing ice hydrolysis and centrifugation to obtain a product for later use; and step D, adding the product in the step C1 into 4 parts of diluted hydrochloric acid with the concentration of 15%, heating to 100 DEG C, hydrolyzing for 3 hours, and cooling to T<40 DEG C to obtain a product. The raw materials are simple and easy to obtain, the cost is low, an intermediate product is non-toxic, and the production efficiency is high.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a preparation method of 2-bromo-5-fluoro-4-nitroaniline. Background technique [0002] 2-Bromo-5-fluoro-4-nitroaniline is an antitumor drug, and most of the existing preparation methods of 2-bromo-5-fluoro-4-nitroaniline use 3-fluoro-4-nitrobenzoic acid React with sodium azide to generate 3-fluoro-4-nitroaniline, and then obtain the final product through bromination; the market demand for raw material 3-fluoro-4-nitrobenzoic acid in this process is small, and the generation process will Sodium azide is generated, which is highly toxic. Therefore, it is necessary to avoid risks in the use of sodium azide, which makes the production process costly and poor in safety. Contents of the invention [0003] In view of the above problems, in order to solve the deficiencies in the prior art, the present invention provides a preparation method of 2-bromo-5-fluoro-4-nitroaniline. [0004] Techni...

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Problems solved by technology

[0002] 2-Bromo-5-fluoro-4-nitroaniline is an antitumor drug, and most of the existing preparation methods of 2-bromo-5-fluoro-4-nitroaniline use 3-fluoro-4-nitrobenzoic acid React with sodium azide to generate 3-fluoro-4-nitroaniline, and then obtain the final product through bromination; the market demand for raw material 3-fluoro-4-nitrobenzoic acid in this process is small, and the generation process will Sodium azide is generated, which is highly toxic. Therefore, it is necessary to avoid the risks in the use of sodium azide, which makes the production process costly and poor in safety.

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