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Efficient synthesizing method of prothioconazole intermediate 1-acetyl-1-cyclopropanoyl chloride

A technology of chlorocyclopropane and prothioconazole, which is applied in the field of synthesis of prothioconazole intermediate 1-acetyl-1-chlorocyclopropane, which can solve the problem of large heat release, difficulty in meeting product yield and quality requirements, It is difficult to control the temperature and other problems, so as to achieve the effect of short reaction time

Inactive Publication Date: 2018-11-13
YANGZHOU TIANCHEN FINE CHEM
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Problems solved by technology

[0002] 1-acetyl-1-chlorocyclopropane is an important intermediate of prothioconazole, due to its low yield, tar affects the quality of the whole product
Usually, the mixture of 3,5-dichloro-2-pentanone and the catalyst is added to the sodium hydroxide solution at 90°C, but the heat of this step is large, and the temperature is difficult to control. After the reaction, a lot of tar is produced. , and 1-acetyl-1-chlorocyclopropane will also deteriorate in contact with sodium hydroxide for a long time, making the yield and quality of the product difficult to meet the requirements

Method used

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Examples

Experimental program
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Effect test

Embodiment Construction

[0006] Take 97g of sodium methoxide (content 25%) in a four-neck flask, stir at room temperature, then slowly drop 58g of 3,5-dichloro-2-pentanone into the flask with a constant pressure dropping funnel, there is a slight exotherm, After dripping, stir at room temperature for 10 min.

[0007] GC detected that the reaction of the raw materials was complete, and the mixture was separated by standing to obtain 41 g of 1-acetyl-1-chlorocyclopropane.

[0008] To measure, the product yield is 92.8%, and the purity is 98%.

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Abstract

The invention discloses an efficient synthesizing method of prothioconazole intermediate 1-acetyl-1-cyclopropanoyl chloride and relates to the technical field of the synthesis of the prothioconazole intermediate 1-acetyl-1-cyclopropanoyl chloride. The method has the advantages that the strong alkalinity of sodium methoxide is utilized to allow raw material 3,5-dichloro-2-pentanone to have ring-closing reaction, the reaction process can be completed under normal temperature and normal pressure, the mole yield of the prothioconazole intermediate 1-acetyl-1-cyclopropanoyl chloride can reach 95%,the synthesized prothioconazole intermediate 1-acetyl-1-cyclopropanoyl chloride is pure, basically no tar is generated, the prothioconazole intermediate 1-acetyl-1-cyclopropanoyl chloride can be usedfor next-step reaction after direct layering, the method is short in reaction time, complete reaction only needs five minutes, and catalyst adding is not needed.

Description

technical field [0001] The invention relates to the technical field of synthesis of prothioconazole intermediate 1-acetyl-1-chlorocyclopropane. technical background [0002] 1-acetyl-1-chlorocyclopropane is an important intermediate of prothioconazole. Due to its low yield, tar affects the quality of the whole product. Usually, the mixture of 3,5-dichloro-2-pentanone and the catalyst is added to the sodium hydroxide solution at 90°C, but the heat of this step is large, and the temperature is difficult to control. After the reaction, a lot of tar is produced. , and 1-acetyl-1-chlorocyclopropane will also deteriorate in contact with sodium hydroxide for a long time, so that the yield and quality of the product are difficult to meet the requirements. Adopt the method of the present invention to synthesize 1-acetyl-1-chlorocyclopropane, because sodium methoxide is alkaline enough, and there is no hydroxide group, can make 3,5-dichloro-2-pentanone ring-closed very effectively, ...

Claims

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Application Information

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IPC IPC(8): C07C45/61C07C49/327
CPCC07C45/61C07C49/327
Inventor 陈国云蔡磊王智峰沈航余耀
Owner YANGZHOU TIANCHEN FINE CHEM
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