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Synthetic method of 2,4-dichloroacetophenone

A technology of dichloroacetophenone and a synthesis method, which is applied in the field of pharmaceutical intermediates 2, can solve the problems such as the lack of clear data on the effect of the electrophilic substitution reaction of m-dichlorobenzene, and achieves convenient operation, simple process, and single acetic anhydride. low consumption effect

Inactive Publication Date: 2019-01-22
XINCHANG COUNTY TAIRU TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent has no clear data on the specific reaction effect of the electrophilic substitution reaction of m-dichlorobenzene

Method used

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  • Synthetic method of 2,4-dichloroacetophenone
  • Synthetic method of 2,4-dichloroacetophenone
  • Synthetic method of 2,4-dichloroacetophenone

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Put acetic anhydride in a dry 500ml four-necked flask equipped with a stirring paddle, a thermometer, a constant pressure dropping funnel, and a rectification tower: 200.0g, anhydrous AlCl 3 : 100.0g. Add m-dichlorobenzene: 100.0 g (98.3%, 0.6687 mol) into the constant pressure dropping funnel. The outer wall of the four-necked flask was kept warm with a water bath, and the temperature of the hot water in the water bath was set at 55°C. Turn on stirring, turn on the vacuum at the top of the rectification tower, and adjust the vacuum at the top of the rectification tower to ≥0.085MPa. When the internal temperature reaches 40°C, slowly add the m-dichlorobenzene in the constant pressure dropping funnel into the four-neck flask dropwise, and the dropping time is controlled within 0.5-1.0 hours. During the dropwise addition process, reflux slowly appears at the top of the rectification tower, and the acetic acid formed by the reaction is extracted by controlling the reflux...

Embodiment 2

[0035] Add acetic anhydride: 112.0g, anhydrous AlCl 3 : 95.0g. Add m-dichlorobenzene: 100.0 g (98.3%, 0.6687 mol) into the constant pressure dropping funnel. The outer wall of the four-necked flask was kept warm with a water bath, and the temperature of the hot water in the water bath was set at 55°C. Turn on stirring, turn on the vacuum at the top of the rectification tower, and adjust the vacuum at the top of the rectification tower to ≥0.085MPa. When the internal temperature reaches 40°C, slowly add the m-dichlorobenzene in the constant pressure dropping funnel into the four-neck flask dropwise, and the dropping time is controlled within 0.5-1.0 hours. During the dropwise addition process, reflux slowly appears at the top of the rectification tower, and the acetic acid formed by the reaction is extracted by controlling the reflux ratio of 1-5:1. After the dropwise addition, raise the temperature of the hot water in the water bath to 80-90°C, reduce the vacuum at the top ...

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PUM

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Abstract

The invention discloses a synthetic method of 2,4-dichloroacetophenone, and the 2,4-dichloroacetophenone is prepared by carrying out electrophilic substitution reaction on m-dichlorobenzene and aceticanhydride as raw materials. According to the method, the electrophilic substitution reaction is carried out by adopting a reaction rectification mode, and the vacuum degree of a reaction rectifying tower is adjusted, and the temperature of the reaction rectifying tower is controlled at optimal temperature for reaction rectification. The single consumption of a catalyst is reduced, the single consumption of the acetic anhydride is reduced, and the production process is simplified.

Description

technical field [0001] The invention relates to the field of fine organic chemical synthesis, in particular to a method for synthesizing a pharmaceutical intermediate 2,4-dichloroacetophenone. Background technique [0002] 2,4-Dichloroacetophenone, English name: 2,4-Dichloroacetophenone, is an important pharmaceutical intermediate, mainly used in the synthesis of antifungal drug ketoconazole. [0003] 2, the chemical synthesis reaction of 4-dichloroacetophenone is as follows: [0004] Reaction equation [0005] [0006] In 2004, Guo Yonghua of Zhejiang University published an article entitled "Synthesis of 2,4-Dichloroacetophenone" in "Chemical Reaction Engineering and Technology". In this paper, carbon disulfide was used as the reaction solvent, anhydrous AlCl 3 As a catalyst, acetyl chloride is used as an acylating agent, and the electrophilic substitution reaction occurs under the condition of controlling the internal temperature at 15°C, which can achieve high sele...

Claims

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Application Information

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IPC IPC(8): C07C45/46C07C49/807
CPCC07C45/46C07C49/807Y02P20/10
Inventor 赵德英
Owner XINCHANG COUNTY TAIRU TECH CO LTD
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