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A kind of preparation method of 4,4'-difluorobenzophenone

A technology of difluorobenzophenone and difluorophenylmethylene chloride, which is applied in the field of preparation of 4,4'-difluorobenzophenone, which can solve the problem of unsatisfactory yield, many steps, and difficult process control, etc. problem, to achieve the effect of low cost, good selectivity and simple process

Active Publication Date: 2018-09-25
大连鼎燕医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0024] The total yield of the three-step reaction reaches 84.5%. However, there are many steps in this process, the process is difficult to control, and the yield is not ideal.

Method used

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  • A kind of preparation method of 4,4'-difluorobenzophenone
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  • A kind of preparation method of 4,4'-difluorobenzophenone

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Embodiment 1

[0035] A kind of preparation method of 4,4'-difluorobenzophenone, described preparation method comprises the steps:

[0036] ① Mix 200g of fluorobenzene and 65g of anhydrous aluminum trichloride, cool to 0-5°C, add 100g of p-fluorobenzotrichloride dropwise and react for 20min to obtain 4,4'-difluorophenyldichloromethane;

[0037] ②Add 4,4'-difluorophenylmethylene chloride to 600g of water and mix well, heat to azeotropic temperature and recover 140g of fluorobenzene, react for 5h, cool to room temperature, filter, dry to obtain 102g of light yellow solid crude product, use 200g of methanol was recrystallized, filtered, washed, and dried to obtain 92g of white crystals with a melting point of 107-108°C. The purity was 99.9% by gas chromatography, and the yield was 90%. through 1 H-NMR detection: δ7.28 (4H, t, hydrogen at the ortho-position of fluorine on the benzene ring); δ7.81 (4H, m, hydrogen at the ortho-position of carbonyl on the benzene ring), consistent with 4,4'-diflu...

Embodiment 2

[0039] A kind of preparation method of 4,4'-difluorobenzophenone, described preparation method comprises the steps:

[0040] ①Mix 100g of p-fluorobenzotrichloride and 200g of anhydrous fluorobenzene, cool to 0-5°C, add 70g of anhydrous aluminum chloride in batches and react for 20min to obtain 4,4'-difluorophenyldichloromethane ;

[0041] ②Add 4,4'-difluorophenyldichloromethane to 600g of water and mix well, heat to azeotropic temperature and recover 139.2g of fluorobenzene, react for 5h, cool to room temperature, filter and dry to obtain 102.8g of light yellow solid crude product , using 200g of methanol for recrystallization, filtering, washing, and drying to obtain 93g of white crystals with a melting point of 107-108°C, the purity of which was 99.9% by gas chromatography, and the yield was 91%. through 1 H-NMR detection: δ7.28 (4H, t, hydrogen at the ortho-position of fluorine on the benzene ring); δ7.81 (4H, m, hydrogen at the ortho-position of carbonyl on the benzene r...

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Abstract

The invention relates to a preparation method of 4,4'-difluorobenzophenone, belonging to the field of chemical synthesis. The preparation method comprises the steps of carrying out acylation reaction on fluorine benzotrichloride and fluorobenzene under the catalysis of aluminum trichloride, and carrying out hydrolysis reaction, so as to obtain 4,4'-difluorobenzophenone. The preparation method of 4,4'-difluorobenzophenone has the beneficial effects of simple process, high yield, good selectivity and low cost.

Description

technical field [0001] The invention relates to a preparation method of 4,4'-difluorobenzophenone, which belongs to the field of chemical synthesis. Background technique [0002] 4,4'-Difluorobenzophenone is the main intermediate for the preparation of engineering plastic polyether ether ketone (PEEK). Polyetheretherketone (PEEK) is a semi-crystalline aromatic plastic engineering plastic with high heat resistance, radiation resistance, corrosion resistance, high impact strength, good wear resistance and fatigue resistance, excellent flame retardancy and electrical properties With its excellent physical and mechanical properties, it can replace metals, ceramics and other materials in many fields. It is one of the most popular high-performance engineering plastics today. It has been widely used in various fields such as coatings and coatings, and has become an indispensable key material. [0003] However, the preparation cost of 4,4'-difluorobenzophenone, the key intermediat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/42C07C49/813
CPCC07C45/42C07C49/813
Inventor 南海军张绥英蔡鲁伯吕永智王洋吴冬辉范莉莉孙立芹
Owner 大连鼎燕医药化工有限公司
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