120983-72-4Relevant articles and documents
AN INDUSTRIAL SCALE PROCESS FOR THE PREPARATION OF PROTHIOCONAZOLE
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Page/Page column 10, (2021/04/23)
The present invention relates to an industrial scale process for the preparation of Prothioconazole (I), which is simple, economical, efficient, user and environment friendly, moreover commercially viable with higher yield and greater chemical purity.
Preparation method 2 - chloro -1 - (1 - chlorocyclopropyl) ethanone
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Paragraph 0032-0047, (2021/01/25)
The invention discloses a preparation method of 2-chloro-1-(1-chlorocyclopropyl)ethanone. The method comprises the steps as follows: in the presence of a Lewis acid salt catalyst and a quaternary ammonium salt phase transfer catalyst, chlorine is introduced into a solvent system with 1-acetyl-1-chlorocyclopropane dissolved or directly introduced into 1-acetyl-1-chlorocyclopropane, the reaction temperature is controlled at 5-25 DEG C for chlorination, and 2-chloro-1-(1-chlorocyclopropyl)ethanone is prepared. 2-chloro-1-(1-chlorocyclopropyl)ethanone prepared with the method has the advantage that content and molar yield can reach 90% or higher.
AZOLE DERIVATIVES, AND AGRICULTURAL AND HORTICULTURAL CHEMICALS AND INDUSTRIAL MATERIAL PROTECTING AGENTS
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Paragraph 0124, (2021/02/13)
To provide plant disease control agents that have low toxicity to humans and animals and excellent handling safety, and exhibit excellent control effect on a variety of plant diseases and high antibiotic action on plant disease germs.SOLUTION: An azole derivative according to the present invention is a compound represented by the formula (I) in the figure, or an N-oxide or agriculturally and pharmaceutically acceptable salt thereof.SELECTED DRAWING: None
One-pot method for synthesizing 1 -chloro -1 - chloroacetyl-cyclopropane
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Paragraph 0020-0032, (2021/05/12)
The invention provides a method for synthesizing 1-chloro-1-chloroacetyl-cyclopropane by adopting one-pot reaction. The synthetic method adopted by the invention is a method for synthesizing the 1-chloro-1-chloroacetyl-cyclopropane by adopting one-pot reaction. The method is short in steps, low in usage of equipment, moderate in operation condition, high in product selectivity and simple in after-treatment, can be used for preparing the 1-chloro-1-chloroacetyl-cyclopropane of which the content is 97% by distillation, and has an industrial production prospect.
Preparation method of 1-chloro-1-chloroacetyl cyclopropane
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Paragraph 0037; 0038, (2020/04/17)
The invention provides a preparation method of 1-chloro-1-chloroacetyl cyclopropane. The preparation method comprises the following steps: 1)reacting 1, 3-butadiene with diazomethane to generate vinylcyclopropane; 2)reacting the vinyl cyclopropane with an oxidation reagent to generate acetyl cyclopropane; and 3)reacting the acetyl cyclopropane with a chlorination reagent to generate the target product 1-chloro-1-chloroacetyl cyclopropane. The method can reduce the use of strong acids, strong bases and chlorination reagents in the preparation of the 1-chloro-1-chloroacetyl cyclopropane, thereby reducing the discharge of three wastes and lowering the safety risk, and can enhance the synthesis yield to adapt to industrial production.
Application of sulfonyl type compounds as chlorination reagent
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Paragraph 0036-0049, (2020/08/27)
The invention discloses an application of a sulfonyl type compound as a chlorination reagent. The structural formula of the sulfonyl type compound is shown as the following formula (I); in formula (I), the R is a substituted or unsubstituted linear or branched alkyl group with 1 to 30 carbon atoms, which means that the alkyl group can be substituted by halogen, alkoxy with 1 to 20 carbon atoms andaryl with 6 to 14 carbon atoms, and the aryl with 6 to 14 carbon atoms can be further substituted by alkyl with 1 to 20 carbon atoms, alkoxy with 1 to 20 carbon atoms and halogen. The sulfonyl compound can perform single chlorination on carbonyl alpha-sites of organic molecules such as aldehyde, ketone, esters and the like with high selectivity under mild conditions; so that the compound can solve the safety problem of existing chlorination reagents such as chlorine, sulfonyl chloride and the like in the use process, reduces post-treatment and three-waste treatment steps, and is suitable forindustrial-scale production.
Method for preparing 1-chloro-1-(chloroacetyl) cyclopropane
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Paragraph 0032; 0068-0077, (2020/12/30)
The invention provides a method for preparing 1-chloro-1 (chloroacetyl) cyclopropane by using a microchannel reactor. The method comprises the steps of B) reacting 1, 3, 5-trichloro-2-pentanone with an alkali liquor in a solvent at a temperature of -5 to 10 DEG C and a pressure of 1.0 to 10.0 bar in the microchannel reactor for 5 to 30 minutes to obtain 1-chloro-1 (chloroacetyl) cyclopropane. Themethod disclosed by the invention is good in selectivity, high in conversion rate and high in product purity, and eliminates polysubstitution byproducts from a reaction source; the method is free of high-temperature and high-pressure reaction and convenient to operate; and moreover, the amplification effect of the reaction is small, and industrial production is facilitated.
Preparation method of 2-chloro-1-(1-chlorocyclopropyl) acetone
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Paragraph 0029; 0033; 0034; 0038; 0039; 0043; 0044; 0048, (2019/05/28)
The invention relates to the technical field of chemical synthesis, and particularly discloses a preparation method of 2-chloro-1-(1-chlorocyclopropyl) acetone. The preparation method comprises the following steps: enabling alpha-acetyl-gamma butyrolactone and hydrochloric acid to have an open-loop decarboxylic reaction to obtain 5-chloro-2-pentanone; adding the 5-chloro-2-pentanone and a catalystinto an alkaline solution, implementing a cyclization reaction, obtaining cyclopropyl methyl ketone; implementing a chlorination reaction with a chloride agent to obtain the 2-chloro-1-(1-chlorocyclopropyl) acetone. The reaction steps of the provided method are less, the reaction period is short, the yield is more than 70%, and the content of the 2-chloro-1-(1-chlorocyclopropyl) acetone in a product is more than 95%.
Synthesis method of 1-chloro-1-chloroacetyl cyclopropane
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Paragraph 0008; 0020, (2018/11/03)
The invention discloses a synthesis method of 1-chloro-1-chloroacetyl cyclopropane. The synthesis method adopts sodium hydroxide, tetrabutylammonium bromide, 3,5-dichloro-2-pentanone, 1-chloro-1-acetyl cyclopropane and sulfuryl chloride as main raw materials. The synthesis method disclosed by the invention has the beneficial effects that the 3,5-dichloro-2-pentanone is heated under the catalytic action of a catalyst and under the alkaline condition to generate elimination reaction. Halogens on primary carbon are easier to remove than halogens on secondary carbon, and when the elimination reaction occurs, chlorine on the 5 position is removed; hydrogen on the 3 position is carbonyl alpha hydrogen and is easier to remove than hydrogen on the 4 position, so that hydrogen on the 3 position isremoved, i.e., the generated gamma elimination reaction. The synthesis method disclosed by the invention has the beneficial effects that by selection of the catalyst, the selectivity of reaction is improved; by monitoring the starting point of secondary reaction, the content of impurities in reaction products is well reduced, so that the purity and the yield of the product are improved.
Synthesis method of 2-chlorine-1-(1-chlorine cyclopropyl) aceton
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Paragraph 0021; 0022; 0023; 0025; 0026; 0028; 0029; 0031, (2018/10/11)
The invention relates to the technical field of synthesis of prothioconazole organic intermediates, in particular to a synthesis method of 2-chlorine-1-(1-chlorine cyclopropyl) aceton. The synthesis method comprises the following steps: putting a certain amount of 1-(1-chlorine cyclopropyl) aceton, dichloromethane and methyl alcohol into a reaction kettle, cooling the mixture to 0 DEG C, startingto feed chlorine into the system, keeping the reaction temperature less than 5 DEG C, stopping feeding the chlorine till the content of the 1-(1-chlorine cyclopropyl) aceton is less than 2 percent, and performing heat preservation reaction for 30 min; at the end of the reaction, firstly extracting residual chlorine and hydrogen chloride from the system at negative pressure for 1 h, performing reduced pressure distillation under the conditions of 25 DEG C and -0.1 MPa to remove the solvent dichloromethane and the catalyst methyl alcohol from the system. According to the synthesis method disclosed by the invention, the chlorine replaces a chloride agent such as sulfonyl chloride, so that production of sulfur dioxide is avoided; the methyl alcohol is used as the catalyst, so that waste waterproduced by use of the lewis acid is avoided; after being recycled, the organic solvent can be continuously used; the posttreatment is simple; the reaction cost is reduced; generation of waste water,waste gas and industrial residues is reduced; the environment can be well protected.
