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Synthesis method of 2, 4-dichloroacetophenone

A technology of dichloroacetophenone and synthesis method, applied in 2 fields, can solve problems such as large amount of waste water, equipment corrosion, serious environmental pollution, etc., and achieve the effect of improving conversion rate and reducing by-products

Inactive Publication Date: 2020-05-08
长沙鑫本助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some enterprises have made great improvements in equipment and the use of rectification towers can achieve higher selectivity and yield, but the use of aluminum chloride not only causes serious equipment corrosion, but also has a large amount of waste water and pollutes the environment. serious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1, 300 grams (Bmim) of Cl-FeCl3 ionic liquid was added to a 1000ml four-necked reaction flask with stirring, reflux condenser and thermometer, and 147 grams (1.0mol) of m-dichlorobenzene and 94.2 grams of m-dichlorobenzene were added under stirring (1.2mol) Acetyl chloride, stirred and heated up, kept at 50°C±2°C for 4 hours, extracted with 200 ml×2 cyclohexane after the reaction, combined the organic phases, evaporated the solvent under reduced pressure to obtain liquid 2,4-di Chloroacetophenone 181.1 grams, purity 97.6%, yield 95.8%. The ionic liquid was washed with cyclohexane and dried for use.

Embodiment 2

[0012] Example 2, 300 grams (Bmim) of Cl-FeCl3 ionic liquid was added to a 1000ml four-necked reaction flask with stirring, reflux condenser and thermometer, and 147 grams (1.0mol) of m-dichlorobenzene and 94.2 grams of m-dichlorobenzene were added under stirring (1.2mol) acetyl chloride, stirred and heated up, and kept at 60°C±2°C for 4h reaction, after the reaction was completed, extracted twice with 200 ml cyclohexane, combined the organic phase, evaporated the solvent under reduced pressure to obtain liquid 2,4- Dichloroacetophenone 181.5 grams, content 96.9%, yield 96.0%. The ionic liquid was washed with cyclohexane and dried for use.

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PUM

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Abstract

The invention discloses a synthesis method of 2, 4-dichloroacetophenone. The method comprises the following steps: carrying out electrophilic substitution reaction on m-dichlorobenzene and acetyl chloride in an ionic liquid (Bmin)Cl-FeCl3 medium to synthesize the 2, 4-dichloroacetophenone; adding m-dichlorobenzene and acetyl chloride into the (Bmin)Cl-FeCl3 ionic liquid according to a molar ratioof 1:(1.1-1.2), carrying out a stirring reaction for 4h at a temperature of 40-60 DEG C, extracting 2, 4-dichloroacetophenone with cyclohexane, and carrying out reduced pressure distillation to removethe solvent so as to obtain 2, 4-dichloroacetophenone. The weight ratio of the feeding amount of the ionic liquid (Bmim)Cl-FeCl3 to the total feeding amount of m-dichlorobenzene and acetyl chloride is 1:(1-0.8). The method has the advantages that the use of anhydrous aluminum chloride is avoided, the conversion rate of raw materials is improved, byproducts are reduced, and green and environment-friendly production is realized.

Description

technical field [0001] The invention relates to the field of organic synthetic chemistry, in particular to a synthesis method of 2,4-dichloroacetophenone. Background technique [0002] 2,4-Dichloroacetophenone is an important fine chemical intermediate, which is widely used in the fields of medicine and pesticides; for example, 2,4-Dichloroacetophenone can be used to synthesize the anti-deep fungal infection drug Flucan azole and itraconazole; can also synthesize low-toxic, broad-spectrum, systemic fungicides teconazole, metroconazole, etoconazole, propiconazole. At present, most of the synthesis of 2,4-dichloroacetophenone is based on m-dichlorobenzene and acetyl chloride or acetic anhydride as raw materials, and the acetylation reaction is carried out under the catalysis of Lewis acid aluminum chloride to obtain 2,4-dichloroacetophenone. Acetophenone. Although some enterprises have made great improvements in equipment and the use of rectification towers can achieve highe...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C45/46C07C49/807
CPCC07C45/455C07C45/46C07C49/807Y02P20/54
Inventor 刘建李刚
Owner 长沙鑫本助剂有限公司
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