63141-09-3Relevant articles and documents
Method for synthesizing prothioconazole intermediate 1-(1-chlorocyclopropyl)ethanone
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Paragraph 0021-0036, (2021/07/08)
The invention relates to a method for synthesizing a prothioconazole intermediate, namely 1-(1-chlorocyclopropyl) ethanone, belonging to the technical field of organic synthesis. The method comprises the following steps: adding 3,5-dichloropentanone serving as a raw material into an organic solvent, adding a catalyst and an acid-binding agent at the same time, conducting heating for a reaction until the monitored raw material disappears, and filtering reaction liquid to obtain the intermediate, namely a 1-(1-chlorocyclopropyl)ethanone solution. According to the method, the anhydrous organic solvent is used as the reaction solvent, and an organic base is used as the catalyst, so a reaction system is changed into a homogeneous system, the use of a phase transfer catalyst is reduced, the generation of hydrolysis impurities is avoided, and the prepared reaction liquid can be directly used for the next reaction without post-treatment. As the selected solvent does not contain water, the water content of the obtained reaction liquid is low, the tedious steps of post-treatment and drying for water removal are omitted, and the method has high economical efficiency and environmental protection property.
Synthesis of 1-chloro-1-acetylcyclopropane through a micro-reactor method
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Paragraph 0023; 0027; 0029-0031; 0033; 0035; 0037, (2018/03/07)
The invention relates to the field of synthesis of a prothioconazole intermediate synthesis, and particularly relates to synthesis of 1-chloro-1-acetylcyclopropane through a micro-reactor method. According to the method, tetraethyl ammonium chloride is adopted as a phase transfer catalyst, sodium hydroxide is adopted as a nucleophilic reagent, dichloromethane is adopted as a solvent, reaction rawmaterials are reacted in a reaction plate of a micro-reactor, reaction conditions are mild, reaction time is short, and a safety coefficient is high. After-treatment is simple, and the 1-chloro-1-acetylcyclopropane is prepared through a water washing step, a drying step, and the like. Solvent removal is not needed, thus reducing loss of a target product in an after-treatment process. The final yield is higher than 95%, purity is higher than 98%, and the method is suitable for industrial production.
Synthesis method for 1-chloro-1-acetyl cyclopropane
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Paragraph 0018-0037, (2018/09/13)
The invention discloses a synthesis method for 1-chloro-1-acetyl cyclopropane. The synthesis method is characterized in that 3,5-dichloro-2-pentanone is taken as a raw material, and solvent oil is taken as a solvent to react with a 20% sodium hydroxide aqueous solution under action of a phase transfer catalyst crown ether, fluid separation and distillation can be performed to separate out 1-chloro-1-acetyl cyclopropane. Solvent oil which does not react with a system is added as the solvent, so that reaction is performed in two phases, and therefore, contact time between a product and alkalineis reduced, product purity is improved, and the yield is improved more greatly. Raw material reaction speed can be increased by adding the phase transfer catalyst, separation speed of the product anda water phase in a post-treatment process is quickened by adding the solvent, and dwell time, in the reaction system, of raw materials and product is integrally shortened, so that side reaction is reduced, and selectivity is improved.