- Synthesis of 8-substituted 5H,9H-6-oxa-7-azabenzocyclononene- 10,11- dione- 11-O-methyloximes, a new [1,2]-oxazonine ring system
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Reaction of (2-bromomethyl-phenyl)-methoxyimino-acetic acid methyl ester 4 with oximes 1 in the presence of NaH/DMF yields 8-substituted 5H,9H-6-oxa- 7-aza-benzocyclononene-10,11-dione-11-O-methyloximes 3 together with the expected open chain compounds 2. Some spectroscopic data as well as synthetic and mechanistic aspects of the formation of the novel compounds 3 are discussed. (C) 2000 Elsevier Science Ltd.
- Pascual, Alfons,Ziegler, Hugo,Trah, Stephan,Ertl, Peter,Winkler, Tammo
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Read Online
- Method for preparing trifloxystrobin by adopting microchannel reactor
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The invention belongs to the technical field of organic synthesis, and particularly relates to a method for preparing trifloxystrobin by adopting a microchannel reactor. The method comprises the following steps: dissolving a raw material methyl (E)-2-(2-chloromethylphenyl)-2-methoxyiminoacetate or methyl (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetate and m-trifluoromethyl acetophenone oxime into a solvent; dissolving sodium methoxide in a solvent; and finally, pumping the two solutions into a micro-channel reactor for complete reaction to obtain a trifloxystrobin feed liquid, and carrying out elutriation and recrystallization to obtain the trifloxystrobin product,wherein the content of trifloxystrobin is 99% or above, and the yield of the step can reach 94% or above. The preparation method provided by the invention has the advantages of simple process operation, high product quality, high yield, less three wastes, small environmental pollution, continuous production, safety and the like, and is suitable for industrial production.
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Paragraph 0044-0050; 0058-0064; 0072-0077
(2021/09/04)
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- Preparation method of trifloxystrobin
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The invention discloses a preparation method of trifloxystrobin. The method comprises the following steps: step 1, carrying out ultrasonic reaction on 3-trifluoromethylacetophenone oxime and (E)-2-(2'-bromomethyl phenyl)-2- carbonylacetic acid methyl ester -O-methylketone oxime in the presence of an acid-binding agent and an organic solvent; step 2, after finishing of the reaction, performing filtering to remove solids, performing washing with water, and carrying out reduced pressure distillation to remove a solvent to obtain a trifloxystrobin crude product; and step 3, recrystallizing a trifloxystrobin crude product with a low-polarity organic solvent, prforming filtering and drying to obtain a trifloxystrobin finished product. Compared with the traditional preparation method, the preparation method disclosed by the invention has the beneficial effects that firstly, an ultrasonic reaction instrument is adopted for reaction, and a low-boiling-point solvent is used for replacing a high-boiling-point reaction solvent, so that the production safety of the product is improved; secondly, the preparation method provided by the invention uses an ultrasonic reaction instrument for reaction, so that the reaction time is greatly shortened, the raw material conversion rate is high, the impurity content is obviously reduced; meanwhile, the production efficiency and the purity of the trifloxystrobin product are improved.
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Paragraph 0027-0037
(2020/07/12)
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- AN IMPROVED PROCESS FOR THE PREPARATION OF TRIFLOXYSTROBIN
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The present invention relates to an improved process for the preparation of trifloxystrobin of formula (I), which is simple, economical, efficient, user and environment friendly, moreover commercially viable with higher yield and chemical purity.
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Page/Page column 17
(2019/04/10)
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- Trifloxystrobin and preparation method of intermittent thereof
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The invention relates to a preparation method of trifloxystrobin. Preparation reaction of the trifloxystrobin is as shown in the description, wherein R is selected from C2-C5 linear alkyl or C3-C5 branched alkyl; in bromination reaction, a brominating agent is selected from NBS or 1,3-dibromo-5,5-dimethylhydantoin.
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Paragraph 0098-0101
(2018/12/13)
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- A NOVEL PROCESS FOR THE PREPARATION OF TRIFLOXYSTROBIN
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The present invention relates to a novel process for preparation of methyl (αE)-(α- (methoxyimino)-2-[[[(E)-[1-[3- (trifluoromethyl) phenyl] ethylidene] amino] oxy] methyl] benzeneaceate (Trifloxystrobin) compound of formula (I) in free form or in agro chemically acceptable salt form useful as a pest control agent.The present invention also relates to a novel process for preparation of methyl (2E)-[2-(bromomethyl) phenyl] (methoxyimino) ethanoate of formula (X) intermediate of Trifloxystrobin. [Formula should be inserted here].
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- Trifloxystrobin synthesizing method
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The invention discloses a trifloxystrobin synthesizing method, and relates to the preparation of trifloxystrobin in organic chemicals. The trifloxystrobin synthesizing method comprises the following steps of using hydroxy methyl phenylacetic acid lactone as raw material to react with TBN (tributyrin), absolute methanol and sodium methoxide to obtain (E)-3-keto-4-(isonitroso)isochroman; using the (E)-3-keto-4-(isonitroso)isochroman to react with acetone and potassium carbonate, and dropwise adding the acetone solution of dimethyl sulfate after a large amount of bright yellow solids occurs, so as to obtain (E)-3-keto-4-(methoxyimino)isochroman; dissolving the obtained (E)-3-ketone-4-(methoxyimino)isochroman by methanol, and dropwise adding thionyl chloride under the low-temperature condition to prepare (E)-2-chlororated methyl-alpha-methoxyimino methyl phenylacetate; after the catalysis of 3-(trifluoromethyl)acetophenone and hydroxylamine hydrochloride, using absolute ethyl alcohol and as solvent to obtain light earthy yellow solid (E)-3-(trifluoromethyl)acetophenone oxime; enabling the (E)-2-bromomethyl-alpha-methoxyimino methyl phenylacetate and the (E)- 3-(trifluoromethyl)acetophenone oxime to react in a DMF (dimethyl formamide) solution of the potassium hydroxide, so as to obtain the white solid of trifloxystrobin.
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- AN IMPROVED PROCESS FOR THE SYNTHESIS OF STROBILURIN FUNGICIDES VIZ TRIFLOXYSTROBIN AND KRESOXIM-METHYL
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The present invention relates to an improved process for the synthesis of E-isomer of compound of formula (5). It further relates to the conversion of formula (5), wherein R is H, to Intermediate (I) and subsequently to substantially pure Trifloxystrobin, compound of formula (I) in good yield.
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- Synergistic Active Compound Combinations Comprising Phenyltriazoles
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The present invention relates to novel active compound combinations comprising, firstly, at least one known compound of the formula (I) in which R1 and R2 have the meanings given in the description. and at least one further known active compound from groups (2) to (27) listed in the description, which combinations are highly suitable for controlling animal pests such as insects and unwanted acarids and also phytopathogenic fungi.
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