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Preparation method of p-fluorobenzaldehyde

A technology of p-fluorobenzaldehyde and fluorobenzene, which is applied in the field of preparation of p-fluorobenzaldehyde, can solve the problems of high process temperature and pressure, high equipment requirements, and many solid wastes, and achieve low equipment requirements, reduce production costs, The effect of avoiding security risks

Active Publication Date: 2021-02-12
江苏多森新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, the patent "A Production Method of p-Fluorobenzaldehyde" with the publication number CN1267658A discloses a method for fluorinating p-chlorobenzaldehyde at a high temperature of 140°C to 180°C. Multi-solid waste (potassium fluoride and potassium chloride)
At the same time, Liu Yu published the paper "Synthesis of p-Fluorobenzaldehyde" (Environmental Science and Technology, 2017, 30(6), 33-36), and the US patent "PRODUCTION OF 4-FLUOROBENZALDEHYDE" with the patent number US6455739B1 ("4- The preparation method of fluorobenzaldehyde ") adopts fluorobenzene and carbon monoxide as raw materials, and prepares p-fluorobenzaldehyde by reaction at 60°C-70°C and 2.0-3.5MPa, but the process temperature and pressure are still high, and the equipment is more demanding

Method used

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  • Preparation method of p-fluorobenzaldehyde
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  • Preparation method of p-fluorobenzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of p-fluorobenzaldehyde, the synthetic route of p-fluorobenzaldehyde (II) is as follows:

[0019]

[0020] A preparation method for p-fluorobenzaldehyde, comprising the following steps:

[0021] Add fluorobenzene (I), catalyst anhydrous aluminum chloride and co-catalyst into the reaction kettle, seal it, pressurize it with nitrogen and carbon monoxide to 1.0kg respectively, and replace it, and then introduce carbon monoxide to control the temperature at 30°C and the pressure at 2.0MPa React until carbon monoxide is no longer inhaled. After the reaction is completed, release the pressure to normal pressure. Control 30°C with 10% hydrochloric acid aqueous solution for acid hydrolysis, then wash with water until neutral, and vertical oil-free vacuum precipitation to an internal temperature of 100 Stop at ℃, and rectify to get p-fluorobenzaldehyde (Ⅱ).

[0022] The mass fraction ratio of fluorobenzene (I) to the catalyst is 5:1; the cocatalyst is a ...

Embodiment 2

[0024] A preparation method of p-fluorobenzaldehyde, the synthetic route of p-fluorobenzaldehyde (II) is as follows:

[0025]

[0026] A preparation method for p-fluorobenzaldehyde, comprising the following steps:

[0027] Add fluorobenzene (I), catalyst anhydrous aluminum chloride and co-catalyst to the reaction kettle, seal it, press it with nitrogen and carbon monoxide to 1.0kg respectively, and then replace it, and then introduce carbon monoxide to control the temperature at 40°C and the pressure at 0.8MPa to react Until the carbon monoxide is no longer inhaled, after the reaction is completed, the pressure is released to normal pressure, under the control of 20°C, acid hydrolysis is carried out with 10% hydrochloric acid aqueous solution by mass percentage, then washed with water until neutral, and the vertical oil-free decompression precipitation is carried out to the internal temperature Stop at 100°C, and obtain p-fluorobenzaldehyde (Ⅱ) through rectification.

[00...

Embodiment 3

[0030] A preparation method of p-fluorobenzaldehyde, the synthetic route of p-fluorobenzaldehyde (II) is as follows:

[0031]

[0032] A preparation method for p-fluorobenzaldehyde, comprising the following steps:

[0033] Add fluorobenzene (I), catalyst anhydrous aluminum chloride and co-catalyst into the reaction kettle, seal it, pressurize it with nitrogen and carbon monoxide to 1.0kg respectively, and then replace it, and then introduce carbon monoxide to control the temperature at 50°C and the pressure at 1.2MPa React until carbon monoxide is no longer inhaled. After the reaction is completed, release the pressure to normal pressure. Under the control of 25°C, use 10% hydrochloric acid aqueous solution for acid hydrolysis, then wash with water until neutral, and vertical oil-free decompression precipitation to the inner Stop when the temperature is 100°C, and rectify to obtain p-fluorobenzaldehyde (Ⅱ).

[0034] The mass fraction ratio of fluorobenzene (I) to the catal...

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Abstract

The invention relates to the technical field of organic chemistry, in particular to a preparation method of p-fluorobenzaldehyde, which comprises the following steps: adding fluorobenzene, a catalystand a cocatalyst into a reaction kettle, sealing, respectively pressurizing to 1.0 kg with nitrogen and carbon monoxide in sequence, replacing, finally introducing carbon monoxide to control the temperature at 30-50 DEG C andthe pressure to be 0.8-2.0 MPa to react until no carbon monoxide is sucked, releasing the pressure to normal pressure after the reaction is finished, controlling the temperature to be 20-30 DEG C, carrying out acidolysis by using a hydrochloric acid aqueous solution with the mass percent of 10%, washing to be neutral, carrying out vertical oil-free decompression desolvation until the internal temperature is 100 DEG C, stopping, and rectifying to obtain fluorobenzaldehyde (II) with the yield of 96% or above and the content of 99.0% or above. The preparation method has the beneficial effects that the reaction conditions are relatively mild, and the temperature and pressure required by the reaction are relatively low, so that the requirement on equipment is relativelylow, the production cost of the product is reduced, and the market competitiveness is improved.

Description

Technical field: [0001] The invention relates to the technical field of organic chemistry, in particular to a preparation method of p-fluorobenzaldehyde. Background technique: [0002] 4-Fluorobenzaldehyde is an important fine chemical intermediate, which is used as the main raw material for the synthesis of various pesticides, medicines, surfactants, polymer monomers, and fungicides. For example, it is used in the synthesis of antihypertensive drugs, antipyretic and analgesic anti-inflammatory drugs, anticancer drugs, and muscle relaxants in medicine; it is used in the synthesis of cyfluthrin and flufluthrin in pesticides, and the synthesis of intermediate m-phenoxy p-fluorobenzaldehyde, and the polymer monomer p-fluorostyrene, among which p-fluorostyrene can be widely used in the manufacture of recording materials, thermoplastic resin coatings, liquid crystal materials, etc. [0003] In the prior art, the patent "A Production Method of p-Fluorobenzaldehyde" with the publi...

Claims

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Application Information

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IPC IPC(8): C07C47/55C07C45/50B01J27/135
CPCC07C45/505B01J27/135B01J27/125B01J27/10B01J35/19C07C47/55
Inventor 何子健
Owner 江苏多森新材料科技有限公司
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