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2-bromine-4-tert-butylphenol preparing method

A technology of tert-butylphenol and p-tert-butylphenol, which is applied in the field of preparation of 2-bromo-4-tert-butylphenol, can solve the problems of polluting reagents, poor selectivity and the like, and achieves simple operation and easy reaction. Control, selectivity and good effect

Inactive Publication Date: 2016-02-10
SINOPHARM CHEM REAGENT
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a kind of preparation method of 2-bromo-4-tert-butylphenol, aims to solve the prior art preparation 2-bromo-4-tert-butylphenol using polluting reagents and poor selectivity question

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preparation example Construction

[0023] The embodiment of the present invention provides a preparation method of 2-bromo-4-tert-butylphenol, comprising the following steps:

[0024] S01. Provide raw materials p-tert-butylphenol, bromide salt and chlorite;

[0025] S02. Place the p-tert-butylphenol, bromide and chlorite in an acidic medium for oxidation reaction, the time of the oxidation reaction is 4-8 hours, and the reaction formula is as follows:

[0026]

[0027] Specifically, in the above step S01, the acquisition of the raw materials p-tert-butylphenol, bromide salt and chlorite is not restricted, and can be obtained by self-preparation or market purchase.

[0028] In the embodiment of the present invention, the green and environment-friendly oxidant chlorite and inorganic bromide are used to replace the traditional bromine as the bromine source, which can not only reduce the possibility of environmental pollution, but also improve the selectivity of the reaction, thereby obtaining the yield and 2-b...

Embodiment 1

[0049] A preparation method of 2-bromo-4-tert-butylphenol, comprising the following steps:

[0050] S11. At room temperature, dissolve 1mol p-tert-butylphenol in 300-500ml acetic acid, add 150-250ml water, and add 1.01mol sodium bromide under stirring;

[0051] S12. At room temperature, under stirring, within 1-2 hours, dropwise add 10% sodium chlorite aqueous solution (available chlorine 128, 2.0 sodium bromide equivalents), and stir at room temperature for 4-8 hours.

[0052] The 2-bromo-4-tert-butylphenol product obtained in the embodiment of the present invention has a conversion rate of over 99%, a yield of 97%, and a content of 98.3%.

Embodiment 2

[0054] A preparation method of 2-bromo-4-tert-butylphenol, comprising the following steps:

[0055] S21. At room temperature, dissolve 1mol p-tert-butylphenol in 400ml acetic acid, add 200ml water, and add 1.01mol sodium bromide under stirring;

[0056] S22. At room temperature, under stirring, within 1-2 hours, dropwise add 10% sodium chlorite aqueous solution (available chlorine 128, 2.0 sodium bromide equivalents), and stir at room temperature for 4-8 hours.

[0057] S23. Control the temperature below 60°C, distill the aqueous acetic acid solution under reduced pressure; cool the raffinate to 0-5°C, and precipitate the crude product of 2-bromo-4-tert-butylphenol;

[0058]S24. Filtrate, wash with cold water, and dry to obtain the product 2-bromo-4-tert-butylphenol.

[0059] The 2-bromo-4-tert-butylphenol product obtained in the embodiment of the present invention has a conversion rate of over 99%, a yield of 97%, and a content of 98.3%.

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Abstract

The invention belongs to the field of chemical synthesis and provides a 2-bromine-4-tert-butylphenol preparing method. The method comprises the steps of providing raw materials P-tert-butylphenol, bromate and chlorite; placing P-tert-butylphenol, bromate and chlorite in an acid medium for oxidation reaction, wherein oxidation reaction is conducted for 4-8 h, and equation is shown in the specification. According to the method, the green oxidant and inorganic bromate are adopted as the bromine source, selectivity is high, the conversion rate of obtained 2-bromine-4-tert-butylphenol is as high as 99%, the yield is as high as 97%, environment pollution is avoided, and the environment protection idea is realized. Furthermore, operation is easy, reaction is easy to control, reaction time is short, the technology is reliable, and industrialization is facilitated.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a preparation method of 2-bromo-4-tert-butylphenol. Background technique [0002] As an important chemical reagent, 2-bromo-4-tert-butylphenol has attracted much attention for its preparation. In the existing literature, for the synthesis method of 2-bromo-4-tert-butylphenol, bromine is mostly used as the bromine source for preparation. However, on the one hand, the existing technology for preparing 2-bromo-4-tert-butylphenol not only has poor selectivity, low conversion rate and poor purity of the obtained product, but also bromine is easy to pollute the environment, which does not conform to the concept of green environmental protection. Therefore, it is particularly important to develop a highly selective and environmentally friendly synthetic method for 2-bromo-4-tert-butylphenol. Contents of the invention [0003] The object of the present invention is to provide a kind...

Claims

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Application Information

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IPC IPC(8): C07C39/27C07C37/62
CPCC07C37/62C07C39/27
Inventor 郭建国刘征宙郑琦孙蔚晨
Owner SINOPHARM CHEM REAGENT