- AN INDUSTRIAL SCALE PROCESS FOR THE PREPARATION OF PROTHIOCONAZOLE
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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.
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Page/Page column 10
(2021/04/23)
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- One-pot method for synthesizing 1 -chloro -1 - chloroacetyl-cyclopropane
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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.
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Paragraph 0020-0032
(2021/05/12)
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- Preparation method 2 - chloro -1 - (1 - chlorocyclopropyl) ethanone
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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.
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Paragraph 0032-0047
(2021/01/25)
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- AZOLE DERIVATIVES, AND AGRICULTURAL AND HORTICULTURAL CHEMICALS AND INDUSTRIAL MATERIAL PROTECTING AGENTS
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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
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Paragraph 0124
(2021/02/13)
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- Method for preparing 1-chloro-1-(chloroacetyl) cyclopropane
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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.
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Paragraph 0032; 0068-0077
(2020/12/30)
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- Preparation method of 1-chloro-1-chloroacetyl cyclopropane
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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.
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Paragraph 0037; 0038
(2020/04/17)
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- Application of sulfonyl type compounds as chlorination reagent
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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.
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Paragraph 0036-0049
(2020/08/27)
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- Preparation method of 2-chloro-1-(1-chlorocyclopropyl) acetone
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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%.
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Paragraph 0029; 0033; 0034; 0038; 0039; 0043; 0044; 0048
(2019/05/28)
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- Synthesis method of 1-chloro-1-chloroacetyl cyclopropane
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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.
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Paragraph 0008; 0020
(2018/11/03)
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- Synthesis method of 2-chlorine-1-(1-chlorine cyclopropyl) aceton
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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.
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Paragraph 0021; 0022; 0023; 0025; 0026; 0028; 0029; 0031
(2018/10/11)
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- Method for preparing 1-chlorine-1'-chloracetyl cyclopropane with trichloroisocyanuric acid as chlorination agent
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The invention discloses a method for preparing 1-chlorine-1'-chloracetyl cyclopropane with trichloroisocyanuric acid as a chlorination agent and belongs to the technical field of pesticide intermediates. According to the method, 1-chlorine-1'-acetyl cyclopropane is utilized as a raw material, inorganic salt is utilized as a catalyst in an organic solvent or an inorganic solvent, the trichloroisocyanuric acid is utilized as the chlorination agent to perform chlorination reaction to prepare the1-chlorine-1'-chloracetyl cyclopropane. The method disclosed by the invention utilizes the safe and cheap trichloroisocanuric acid as the chlorination agent, so that pollutant emission in a general chlorination process is reduced, the 1-chlorine-1'-acetyl cyclopropane can react under more moderate condition, reaction selectivity is high, after treatment is simple, and industrial production prospect is achieved.
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Paragraph 0019; 0020
(2017/09/18)
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- Method using micro reactor to prepare 1-chloro-1'-chloroacetyl cyclopropane
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The invention discloses a method using a micro reactor to prepare 1-chloro-1'-chloroacetyl cyclopropane. The reactions can be carried out in the presence or absence of a solvent. According to the preparation method, 1-chloro-1'-acetyl cyclopropane and chlorine gas are pumped into a micro reaction channel to carry out reactions by a feed pump according to a certain ratio. The device comprises a raw material bottle, a feed pump, a pre-heating or pre-cooling pipe, a micro reactor, a time delay pipe, a temperature controlling device, a counterbalance valve, and a product receiver. A micro reactor, which can quickly mix the raw materials and has a good heat exchange effect, is used as the reaction device; so that 1-chloro-1'-acetyl cyclopropane and chlorine gas can carry out high selective(alpha-position hydrogen atom) chlorination reactions in a micro channel under high speed and efficient mixing to generate 1-chloro-1'-chloroacetyl cyclopropane. The provided method has the advantages of simple operation, mild conditions, high selectivity, and low energy consumption; compared with the conventional reactions, the using amount of solvent is reduced, and moreover, the method is environment-friendly and can be easily applied to industrialization.
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Paragraph 0019
(2016/10/20)
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- Fungicidal and plant growth-regulating azolylmethyl-cyclopropyl derivatives
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Fungicidal and plant growth-regulsting azolylmethylcyclopropyl derivatives of the formula STR1 in which R represents halogen, alkyl or optionally substituted phenyl, or represents the groupings --Y--R2, wherein Y represents oxygen, sulphur, SO or SO2 and R2 represents optionally substituted phenyl, R1 represents hydrogen, alkyl or acyl, X represents nitrogen or a CH group, Z represents halogen, alkyl with 1 to 4 carbon atoms, alkoxy with 1 to 4 carbon atoms, alkylthio with 1 to 4 carbon atoms, halogenoalkyl with 1 or 2 carbon atoms and 1 to 5 halogen atoms, halogenoalkoxy with 1 or 2 carbon atoms and 1 to 5 halogen atoms, halogenoalkylthio with 1 or 2 carbon atoms and 1 to 5 halogen atoms or phenyl which is optionally substituted by aklyl with 1 or 2 carbon atoms and/or halogen, or represents phenoxy which is optionally substituted by alkyl with 1 or 2 carbon atoms and/or halogen and m represents the number 0, 1, 2 or 3, and addition products thereof with acids and metal salts. Intermediates therefor of the formulas STR2 are also new.
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- Fungicidal and plant growth-regulating hydroxyethyl-azolyl derivatives
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Fungicidal and plant growth regulating hydroxyethylazolyl derivatives of the formula STR1 in which R represents hydrogen, alkyl or acyl, R1 represents halogen, optionaly substituted phenyl or the grouping --Z--R3, wherein Z represents oxygen, sulphur, SO or SO2 and R3 represents optionally substituted phenyl, R2 represents halogen, alkyl having 1 to 4 carbon atoms, alkoxy having 1 to 4 carbon atoms, alkylthio having 1 to 4 carbon atoms, halogenoalkyl having 1 or 2 carbon atoms and 1 to 5 halogen atoms, halogenoalkoxy having 1 or 2 carbon atoms and 1 to 5 halogen atoms, halogenoalkylthio having 1 or 2 carbon atoms and 1 to 5 halogen atoms, alkoximinomethyl with 1 to 4 carbon atoms in the alkoxy group, phenyl which is optionally substituted by alkyl having 1 or 2 carbon atoms and/or halogen, or phenoxy, which is optionally substituted by alkyl having 1 or 2 carbon atoms and/or halogen, m represents the number 0, 1, 2 or 3, X represents nitrogen or a CH group and Y represents oxygen, sulphur, SO or SO2, and addition products thereof with acids and metal salts. Intermediates of the formulas STR2 are also new.
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