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

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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...

Method used

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Examples

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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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