A kind of preparation method of difenoconazole nitrate
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A technology of difenoconazole and nitrate, applied in directions such as organic chemistry, can solve the problems of many solid wastes, severe reaction conditions, and high reaction temperature, and achieve the effects of improving safety, short reaction time, and increasing the content of crude products
Active Publication Date: 2022-03-01
利民化学有限责任公司
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[0005] In order to solve the shortcomings of the prior art such as high reaction temperature, severe reaction conditions, and many solid wastes, the present invention provides an economical, green and environmentally friendly preparation method for difenoconazole nitrate suitable for industrial production
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Embodiment 1
[0034] Add 2-(bromomethyl)-2-(2-chloro-4-(4-chlorophenoxy)phenyl)-4-methyl-1,3-dioxolane ( 4g, 9.57mmol) and 1H-1,2,4 triazole (0.66g, 9.57mmol), potassium carbonate (1.32g, 9.57mmol), potassium iodide (0.16g, 0.96mmol) and toluene 20mL, placed in microwave reaction The reaction was carried out at 160° C. for 15 minutes in an apparatus, and the reaction yield was 85.2% by liquid phase monitoring.
Embodiment 2
[0036] Add 2-(bromomethyl)-2-(2-chloro-4-(4-chlorophenoxy)phenyl)-4-methyl-1,3-dioxolane ( 4g, 9.57mmol) and 1H-1,2,4 triazole (0.8g, 11.48mmol), potassium carbonate (2.64g, 14.35mmol), potassium iodide (0.40g, 2.39mmol) and N,N-dimethyl Formamide 20mL was placed in a microwave reactor and reacted at 185°C for 15min, and the reaction yield was 92.6% by liquid phase monitoring.
Embodiment 3
[0038] Add 2-(bromomethyl)-2-(2-chloro-4-(4-chlorophenoxy)phenyl)-4-methyl-1,3-dioxolane ( 4g, 9.57mmol) and 1H-1,2,4 triazole (1.0g, 14.35mmol), potassium carbonate (1.98g, 19.14mmol), potassium iodide (0.80g, 4.78mmol) and N-methylpyrrolidone 20mL, Placed in a microwave reactor and reacted at 190°C for 15 minutes, the reaction yield was 91.8% by liquid phase monitoring.
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Abstract
A preparation method of difenoconazole nitrate, comprising the following steps: 2-(bromomethyl)-2-(2-chloro-4-(4-chlorophenoxy)phenyl)-4-methyl Base-1,3-dioxolane and 1H-1,2,4-triazole carry out microwave reaction in the presence of acid-binding agent, catalyst and solvent; obtain the difenoconazole crude product dissolution after distillation; The crude product of difenoconazole is dissolved, and nitric acid is added to form a salt; after filtering and drying, the finished product of difenoconazole nitrate is obtained. The invention has milder reaction conditions for preparing difenoconazole nitrate, shorter reaction time, less solvent consumption, simple steps, environmental protection, suitability for industrialized production, and high yield and content of the final product.
Description
technical field [0001] The invention relates to the field of pesticide preparation, in particular to a method for preparing the fungicide difenoconazole nitrate. Background technique [0002] Difenoconazole (1-((2-(2-chloro-4-(4-chlorophenoxy)phenyl)-4-methyl-1,3-dioxolan-2-yl)methanol Base)-1H-1,2,4-triazole) is a very important triazole agricultural fungicide, has systemic properties, belongs to sterol demethylation inhibitor, and belongs to broad-spectrum fungicide. For Ascomycetes, Basidiomycetes and including Alternaria, Ascodiospora, Cercospora, Spirospora, Ballacne, Phoma, Septoria, Septoria, Semi-known fungi including the genus Scabella, Powdery mildew family, Rust fungi and certain kinds of pathogenic bacteria have lasting protective and therapeutic effects. It has a good curative effect on grape powdery mildew, peanut leaf spot, net spot, potato early blight, wheat glume blight, leaf blight, and rust. [0003] [0004] At present, there are many patents at ho...
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