A kind of pyridylpyrazole-4-carboxamide compound based on sulfur-containing functional group and its preparation method and application
A technology of pyridylpyrazoles and carboxamides, which is applied in the field of pyridylpyrazole-4-carboxamides and their preparation, and achieves the effects of easy operation, simple method and good insecticidal activity
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Embodiment 1
[0066] Example 1: 3-bromo-N-(4-chloro-2-methyl-6-(2-(2-(methylthio)acetyl)hydrazinecarbonyl)phenyl)-1-(3-chloropyridine Preparation of -2-yl)-1H-pyrazole-5-carboxamide
[0067]
[0068] In a 100mL single-necked bottle, the intermediate 3-bromo-N-(4-chloro-2-(hydrazinecarbonyl)-6-methylphenyl)-1-(3-chloropyridin-2-yl)-1H- Pyrazole-5-carboxamide (0.48 g, 1 mmol), methylthioacetic acid (0.10 g, 1.0 mmol) and TBTU (0.35 g, 1.1 mmol) were dissolved in 20 mL of N,N-dimethylformamide (DMF) , stirred at room temperature for 15min, then added TEA (0.30g, 3.0mmol) and continued to stir, reacted for 3h, followed by TLC spot plate, after the raw material point disappeared, pour the reaction solution into 500mL saturated sodium chloride solution, stir for 0.5h, and dissolve the solid Filter, dry, and purify by column chromatography.
Embodiment 2
[0069] Example 2: 3-bromo-N-(4-chloro-2-methyl-6-(2-(2-(methylsulfinyl)acetyl)hydrazinecarbonyl)phenyl)-1-(3- Preparation of chloropyridin-2-yl)-1H-pyrazole-5-carboxamide
[0070]
[0071] In a 100mL single-necked bottle, the intermediate 3-bromo-N-(4-chloro-2-methyl-6-(2-(2-(methylthio)acetyl)hydrazinecarbonyl)phenyl)-1- (3-Chloropyridin-2-yl)-1H-pyrazole-5-carboxamide (0.57g, 1mmol), m-chloroperoxybenzoic acid (MCPBA) (0.21g, 1.0 mmol) was dissolved in 20mL dichloro In methane (DCM), stir under ice bath for 15min, then add sodium bicarbonate (0.25g, 3mmol) and continue to stir, react for 3h, TCL dot plate tracking, after the raw material point disappears, the reaction solution is dried under reduced pressure, column chromatography Purify.
Embodiment 3
[0072] Example 3: 3-bromo-N-(4-chloro-2-methyl-6-(2-(2-(methylsulfonyl)acetyl)hydrazinecarbonyl)phenyl)-1-(3-chloro Preparation of pyridin-2-yl)-1H-pyrazole-5-carboxamide
[0073]
[0074] In a 100mL single-necked bottle, the intermediate 3-bromo-N-(4-chloro-2-methyl-6-(2-(2-(methylthio)acetyl)hydrazinecarbonyl)phenyl)-1- (3-Chloropyridin-2-yl)-1H-pyrazole-5-carboxamide (0.57g, 1mmol), m-chloroperoxybenzoic acid (MCPBA) (0.51g, 2.5mmol) was dissolved in 20mL dichloromethane ( DCM), stirred at room temperature for 15 min, then added sodium bicarbonate (0.25 g, 3 mmol) and continued to stir, reacted for 3 h, followed by TCL spot plate, after the raw material point disappeared, the reaction solution was dried under reduced pressure, and purified by column chromatography.
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