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Synthesis process of 3,5-dichloro-2-pentanone

A synthesis process, technology of pentanone, which is applied in the field of synthesis process of 3,5-dichloro-2-pentanone, can solve problems such as impact and unfavorable industrial operation, and achieve increased purity, reduced loss of hydrochloric acid, and less waste Effect

Active Publication Date: 2017-12-15
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In addition, in the patent CN105461533A published in China and the article "Synthesis of 3,5-dichloro-2-pentanone", it is mentioned that a phase transfer catalyst, a Lewis acid catalyst and a water-carrying agent are used in the reaction, and in the patent CN104292089A In the process, concentrated hydrochloric acid is added dropwise, and organic solvents are needed, which is not conducive to industrial operation
[0008] Known by above-mentioned tradition and existing technology, existing synthetic technology still has various problems, has greatly influenced the synthetic research of 3,5-dichloro-2-pentanone, therefore, to 3,5-dichloro It is of great significance to study and improve the synthesis process of -2-pentanone

Method used

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  • Synthesis process of 3,5-dichloro-2-pentanone
  • Synthesis process of 3,5-dichloro-2-pentanone
  • Synthesis process of 3,5-dichloro-2-pentanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 9 kg of α-acetyl-γ-butyrolactone into a 20L glass reactor equipped with a stirring device and a thermometer, and cool down the reactor with a circulating cold trap. When the reaction temperature drops to 5°C, start to add 9.9 kg of sulfonyl chloride dropwise , adjust the rate of addition to ensure that the reaction temperature is controlled at about 10°C. After the dropwise addition, the insulation reaction is carried out for 0.5h (to obtain the crude product of α'-chloro-α-acetyl-γ-butyrolactone), and the pressure is reduced at room temperature (-0.1MPa ) and stirred for 2h. Then discharge 11.4kg into a 50L heating kettle, then add 11.4kg of water and 22.8kg of 30% hydrochloric acid in sequence, heat the heat transfer oil to 60°C, keep warm for 0.5h, then heat up to 90°C, keep warm for 0.5h, and continue to heat up to 120°C ℃, heat preservation reaction for 8 hours, the circulating cold trap cools the condenser tube (-15℃), and the azeotrope of 3,5-dichloro-2-penta...

Embodiment 2

[0035] Add 9Kg of α-acetyl-γ-butyrolactone in a 20L glass reactor equipped with a stirring device and a thermometer, and cool down the reactor with a circulating cold trap. When the reaction temperature drops to 10°C, start to add 9.9Kg of sulfuryl chloride dropwise. Control the dropping rate, control the reaction temperature at about 10°C, keep the reaction for 0.5h after the dropwise addition, and stir under reduced pressure (-0.1MPa) at room temperature for 2h. Then put the material into a 50L heating kettle, weigh 11.5Kg, then add 11.5Kg of water and 23Kg of 30% hydrochloric acid in sequence, heat the heat transfer oil to 60°C, keep the temperature for 0.5h, then raise the temperature to 90°C, keep the heat for 0.5h, and continue to heat up To 120°C, hold the reaction for 8 hours, cool down the condenser tube with a circulating cold trap (-15°C), obtain the azeotrope of 3,5-dichloro-2-pentanone and water in the water separator, and directly separate the lower organic phase ...

Embodiment 3

[0037] Add 9Kg of α-acetyl-γ-butyrolactone in a 20L glass reactor equipped with a stirring device and a thermometer, and cool down the reactor with a circulating cold trap. When the reaction temperature drops to 5°C, start to add 9.9Kg of sulfuryl chloride dropwise. Control the dropping rate, control the reaction temperature at about 10°C, keep the reaction for 0.5h after the dropwise addition, and stir under reduced pressure (-0.1MPa) at room temperature for 2h. Then feed into the 50L heating kettle, weigh 11.4Kg, then add 11.4Kg of water, 22.8Kg of 30% hydrochloric acid successively, the heat conduction oil is heated up to 120°C, keep warm for 8h, and the circulating cold trap cools the condenser tube (-15°C), and divides The azeotrope of 3,5-dichloro-2-pentanone and water is obtained in the water tank, and the lower organic phase is directly separated into the product collector to obtain 7.1Kg of high-purity 3,5-dichloro-2-pentanone , The crude yield is 65%, the content is ...

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Abstract

The invention discloses a synthesis process of 3,5-dichloro-2-pentanone. The process uses water as a solvent, alpha-acetyl-gamma-butyrolactone undergoes the continuous reaction of sulfonyl chloride chlorination, hydrolysis and ring opening, decarboxylation and re-chlorination in a double-layer glass reaction kettle to obtain the high-purity 3,5-dichloro-2-pentanone. The process adopts a staged temperature-controlled reaction, does not need any catalyst compared with a traditional process, can make the reaction completely performed, is safe and low in cost, is environmentally friendly, meanwhile is high in reaction yield and strong in industrialized operability and has a good application prospect.

Description

technical field [0001] The invention belongs to the field of fine chemical synthesis, and in particular relates to a synthesis process of 3,5-dichloro-2-pentanone. Background technique [0002] 3,5-Dichloro-2-pentanone is a very important intermediate in the synthesis of medicines and pesticides, especially prothioconazole, a new broad-spectrum triazolethione fungicide with outstanding product performance. At present, there are many ways to synthesize 3,5-dichloro-2-pentanone, mainly using α-acetyl-γ-butyrolactone as raw material, and producing it through chlorination, ring opening, decarboxylation and rechlorination. have to. Such as: [0003] (1) Solid phosgene chlorination method, α-acetyl-γ-butyrolactone is chlorinated by chlorine to obtain α'-chloro-α-acetyl-γ-butyrolactone, and then reacted with solid phosgene to obtain 3 ,5-Dichloro-2-pentanone. Although this method reduces the three wastes, the yield is only 81.5%, and solid phosgene is a highly toxic chemical, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/16C07C45/59C07D307/33
CPCC07C45/59C07D307/33C07C49/16
Inventor 韦永飞温兰兰方红新张令伟李文兵赵志华王晓亭
Owner ANHUI COSTAR BIOCHEM CO LTD
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