Synthetic method for 2,4-dichloroacetophenone

A technology of dichloroacetophenone and its synthesis method, which is applied in the field of pharmaceutical intermediates 2, can solve the problem that there is no clear data on the effect of the electrophilic substitution reaction of m-dichlorobenzene, and achieve convenient operation, low unit consumption, and equipment investment little effect

Inactive Publication Date: 2019-05-07
XINCHANG COUNTY TAIRU TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent has no clear data on the specific reaction effec...

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

Examples

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Effect test

Embodiment 1

[0034] Put acetic anhydride: 200.0g, anhydrous AlCl3: 100.0g into a dry 500ml four-necked flask equipped with a stirring paddle, a thermometer, a constant pressure dropping funnel, and a rectification tower. 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

[0037] Put 112.0 g of acetic anhydride and 95.0 g of anhydrous AlCl3 into a dry 500 ml four-necked flask equipped with a stirring paddle, a thermometer, a constant pressure dropping funnel, and a rectification tower. 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 th...

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PUM

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Abstract

The invention discloses a synthetic method for 2,4-dichloroacetophenone. The method comprises the step of performing an electrophilic substitution reaction by using m-dichlorobenzene and acetic anhydride as raw materials to synthesize the 2,4-dichloroacetophenone. According to the method provided by the invention, the electrophilic substitution reaction is performed by adopting a reactive rectification manner, a vacuum degree of a reaction rectification column is adjusted, temperature of the reaction rectification column is controlled, reactive rectification is performed under the optimal temperature condition, so that the catalyst unit consumption and the acetic anhydride unit consumption are 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 is used as the reaction solvent, anhydrous AlCl3 is used as the catalyst, acetyl chloride is used as the acylating agent, and the electrophilic substitution reaction occurs under the condition of controlling the internal temperature at 15°C, which can achieve ...

Claims

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Application Information

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IPC IPC(8): C07C45/46C07C45/82C07C49/807
CPCY02P20/10
Inventor 赵梦炜
Owner XINCHANG COUNTY TAIRU TECH CO LTD
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