A kind of preparation method of fluorine-containing phenol

Abstract

The invention provides a preparation method of fluorine-containing phenol. The preparation method comprises the following steps of: a) mixing a copper catalyst, a ligand, alkali, fluorine-containing bromobenzene and tertiary butanol for esterification reaction to obtain fluorine-containing phenyl tertiary butyl ester; and b) mixing the fluorine-containing phenyl tertiary butyl ester obtained in the step a) with concentrated sulfuric acid and water for hydrolysis reaction to obtain the fluorine-containing phenol. Compared with the prior art, the preparation method provided by the invention directly prepares a fluorine-containing phenyl tertiary butyl ester intermediate by adopting tertiary butanol in a breakthrough manner, and then prepares the fluorine-containing phenol through the hydrolysis reaction. The process route is simple and can be continuously operated, the reaction condition is mild, and the conventional cost of raw materials is low, and the method is suitable for industrial production; moreover, the total yield of the fluorine-containing phenol prepared by the preparation method provided by the invention can reach 76% above, and the product purity is 99% above.

Description

technical field [0001] The invention relates to the technical field of fluorine chemical industry, in particular to a preparation method of fluorine-containing phenol. Background technique [0002] Fluorine-containing phenol is a very important chemical product, especially in the field of fine chemicals, including medicine, pesticides, etc., and has very important application prospects. At the same time, fluorine-containing phenol is also an important liquid crystal material intermediate. The introduction of fluorine atoms into liquid crystal molecules can make liquid crystal materials have the advantages of low viscosity, fast response speed, and high resistivity. Therefore, using fluorine-containing phenol as a liquid crystal material intermediate to develop Fluorine liquid crystal products have very broad prospects. [0003] At present, there are few processes for synthesizing fluorine-containing phenol in the prior art, mainly including: [0004] (1) The Chinese patent...

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Problems solved by technology

[0012] The above method mainly has the following disadvantages: in the method (1), the ammoniation process must be carried out under high temperature and high pressure conditions, while the diazotization reaction uses a strong acid, the reaction conditions are harsh, the equipment requirements are high, and the yield of the entire process route is low; Method (2) requires anhydrous and oxygen-free conditions, and the borate reaction will be carried out at low temperature, and the yield is greatly affected by temperature, and a large amount of solvent is needed simultaneously, and it is not easy to recycle; the organic peroxide used in method (3) is Tert-butyl peroxybenzoate (TBPB), using peroxide as an oxidant, has potential safety hazards, and the reaction produces a large amount of by-product magnesium bromide benzoate without commercial value; method (4) raw materials are not commercial products, and the price Expensive, the reaction produces a large amount of waste water containing by-product boric acid, which is not suitable for industrial production

[0013] Therefore, the above-mentioned methods for preparing fluorine-containing phenols have low yields and complex processes, all of which have relatively large limitations and are difficult to meet the needs of industrialized production.

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