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Synthetic method for 4-fluorobenzaldehyde

A technology for p-fluorobenzaldehyde and a synthesis method, which is applied in chemical instruments and methods, preparation of carbonyl compounds by hydrolysis, preparation of halogenated hydrocarbons, etc., can solve the problems of low recovery rate and difficult requirements for process equipment, and achieves easy operation and environmental protection. The effect of no pollution equipment requirements and mild reaction conditions

Inactive Publication Date: 2014-10-15
SINO HIGH CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of the present invention is to solve the problems of low recovery rate and difficult requirements on process equipment in the production technology of p-fluorobenzaldehyde in the prior art, and provide a kind of synthetic method of p-fluorobenzaldehyde

Method used

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  • Synthetic method for 4-fluorobenzaldehyde
  • Synthetic method for 4-fluorobenzaldehyde
  • Synthetic method for 4-fluorobenzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) 110.5g of p-fluorotoluene is added to 500ml of chloroform, continue feeding chlorine gas in the middle, carry out chlorination reaction, control the progress of the reaction with GC tracking method, make the content of monochlorobenzyl product less than 2%, and the content of trichlorobenzyl product less than 10%,

[0037] (2) Add FeCl to it 3 +ZnCl 2 Catalyst 6.9g, then heat up to 130°C, add 1.7ml of water to initiate the reaction for hydrolysis, control the temperature to reflux at 130°C,

[0038] (3) Add water dropwise in the there-necked flask, make the complete hydrolysis of dichlorobenzyl product,

[0039] (4) After the reaction finishes, adjust the pH value to 8.0~9.0 with a concentration of 30% sodium hydroxide solution, then leave to stand for stratification,

[0040] (5) adding 10% hydrochloric acid to adjust the pH value to 5.0-7.0, adding toluene to extract the organic layer,

[0041] (6) Finally, the solvent was spin-dried, the product was dried, an...

Embodiment 2

[0045] (1) 69g of p-fluorotoluene is added to 500ml of difluorotoluene, continue to feed chlorine gas in the middle, carry out chlorination reaction, control the progress of the reaction with GC tracking method, make the content of monochlorobenzyl product less than 2%, and the content of trichlorobenzyl product less than 2%. 10%,

[0046] (2) Add FeCl to it 3 +ZnCl 2 Catalyst 6.9g, then heat up to 100°C, add 0.5ml of water to initiate the reaction for hydrolysis, control the temperature to reflux at 100°C,

[0047] (3) Add water dropwise in the there-necked flask, make the complete hydrolysis of dichlorobenzyl product,

[0048] (4) After the reaction finishes, adjust the pH value to 8.0~9.0 with a concentration of 30% sodium hydroxide solution, then leave to stand for stratification,

[0049] (5) adding 10% hydrochloric acid to adjust the pH value to 5.0-7.0, adding THF to extract the organic layer,

[0050] (6) Finally, the solvent was spin-dried, the product was dried, ...

Embodiment 3

[0054] (1) 138g of p-fluorotoluene is added to 500ml of difluorotoluene, continue to feed chlorine gas in the middle, carry out chlorination reaction, control the progress of reaction with GC tracking method, make the monochlorobenzyl product content be less than 2%, the trichlorobenzyl product content is less than 10%,

[0055] (2) Add FeCl to it 3 +ZnCl 2 Catalyst 6.9g, then heat up to 150°C, add 5ml of water to initiate the reaction for hydrolysis, control the temperature to reflux at 150°C,

[0056] (3) Add water dropwise in the there-necked flask, make the complete hydrolysis of dichlorobenzyl product,

[0057] (4) After the reaction finishes, adjust the pH value to 8.0~9.0 with a concentration of 30% sodium hydroxide solution, then leave to stand for stratification,

[0058] (5) adding 10% hydrochloric acid to adjust the pH value to 5.0-7.0, adding DMF to extract the organic layer,

[0059] (6) Finally, the solvent was spin-dried, the product was dried, and the organ...

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Abstract

The invention discloses a synthetic method for 4-fluorobenzaldehyde, and belongs to the technical field of chemical synthesis. The synthetic method comprises: taking 4-fluorotoluene as a raw material, performing a chlorination reaction on 4-fluorotoluene and chlorine, so as to generate a benzal chloride product; then under the effect of a composite catalyst of ferric trichloride and zinc chloride, performing heating hydrolysis on the benzal chloride product; and finally after hydrolysis is finished, performing extraction and rectification to obtain 4-fluorobenzaldehyde. The synthetic method has the advantages of less synthetic steps, high reaction yield (77% or more), mild reaction conditions, simple operation, environment friendliness, no pollution, not high equipment requirement, suitableness for industrialization production, and the like.

Description

【Technical field】 [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthetic method of p-fluorobenzaldehyde. 【Background technique】 [0002] P-Fluorobenzaldehyde is an important intermediate in organic synthesis, which can be used in the synthesis of medicines, such as antihypertensive drugs, antipyretic, analgesic and anti-inflammatory drugs, anticancer drugs, muscle relaxants, etc. The earliest synthesis methods of p-fluorobenzaldehyde include the oxidation of p-fluorotoluene, the oxidation of p-fluorobenzyl alcohol or p-fluorophenylacetic acid, and the reduction of p-fluorobenzonitrile. Due to the instability of the intermediates used, the poisonous hydrogen fluoride raw materials, and many synthetic steps, these methods have made little progress in industrial development and research, and seem to be unable to be used in large-scale industrial production. In recent years, Japan, the United States, etc. have realized the import...

Claims

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Application Information

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IPC IPC(8): C07C45/43C07C47/55
CPCC07C45/43C07C17/14
Inventor 冯志强严留新汤浩
Owner SINO HIGH CHINA
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