A substituted pyrazolylpyrazolesulfonylurea compound or its salt acceptable as a pesticide, composition and use thereof
A technique for pyrazolylpyrazolesulfonylureas and compounds, which is applied in the fields of chemicals, applications, organic chemistry, etc. for biological control, and can solve the problems of undisclosed pyrazolesulfonylurea compounds and compounds with insufficient activity , to achieve the effect of good selectivity and safety, good activity and selectivity
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Embodiment 1
[0097] 2-(N-((1-(3-Cl-4,5,6,7-tetrahydropyrazolo[1,5A]pyridin-2-yl)4-cyano-1H-pyrazole-5- base) carbamoyl) sulfonamide) methyl benzoate (compound 1) synthesis:
[0098]
[0099] Add 5-amino-1-(3-chloro-4,5,6,7-tetrahydropyrazolo[1,5-A]pyridin-2yl)-1H-pyrazole-4-methanol to the reaction flask Nitrile 2.62g (10mmol), acetonitrile 30mL, 2-sulfonyl isocyanate methyl benzoate 2.4g (10mmol) was added under stirring, stirred at room temperature for 6h, TLC followed the reaction (ethyl acetate:petroleum ether=1:1, GF254 , UV color development), after the reaction was complete, spin out the solvent, and purify the compound by column chromatography to obtain 3.15 g of the target compound, a white solid powder, melting point: 110-112 ° C; 1 H-NMR (CDCl 3 -d 6 ,500MHz)δ:8.12-8.09(m,1H),7.79-7.76(s,1H),7.72-7.69(m,1H),7.48-7.54(m,2H),4.34-4.30(t,2H), 3.90-3.86 (s, 3H), 2.73-2.69 (t, 2H), 1.73-1.69 (m, 2H), 1.46-1.42 (m, 2H).
Embodiment 2
[0101] 2-(N-((1-(3-Cl-4,5,6,7-tetrahydropyrazolo[1,5A]pyridin-2-yl)4-cyano-1H-pyrazol-5yl ) carbamoyl) sulfonamide) benzoic acid synthesis (compound 2):
[0102]
[0103] Add 2-(N-((1-(3-Cl-4,5,6,7-tetrahydropyrazolo[1,5A]pyridin-2-yl)4-cyano-1H- Pyrazole-yl) carbamoyl) sulfonamide) methyl benzoate 5.03g (10mmol), methanol 30mL, add sodium hydroxide 0.41g (1.1mmol), water 1mL under stirring, stir at room temperature for 6h, follow the reaction by TLC (Ethyl acetate:petroleum ether=1:1, GF254, UV color development), after the reaction is complete, spin out the solvent, add 50mL dichloromethane, 10mL saturated saline, separate layers, and spin dry the solvent; column chromatography purifies the compound , to obtain 2.93g of the target compound, light yellow solid powder, melting point: 111-113°C; 1 H-NMR (CDCl 3 -d 6 ,500MHz)δ:8.18-8.14(d,1H),8.09-8.06(d,1H),7.91-7.88(s,1H),7.72-7.68(m,2H),4.25-4.23(t,2H), 2.82-2.78 (t, 2H), 2.11-2.07 (m, 2H), 1.97-1.92 (m, 2H).
Embodiment 3
[0105] Synthesis of compound 3:
[0106]
[0107] Add 5-amino-1-(3-chloro-4,5,6,7-tetrahydropyrazolo[1,5-A]pyridin-2yl)-1H-pyrazole-4carbonitrile into the reaction flask 2.62g (10mmol), 30mL of acetonitrile, 2.6g (10mmol) of methyl 2-((isocyanatesulfonyl)methyl)benzoate was added under stirring, the reaction was stirred at room temperature for 6h, and the reaction was tracked by TLC (ethyl acetate:petroleum ether= 1:1, GF254, UV color development), after the reaction is complete, spin out the solvent, and purify the compound by column chromatography to obtain 3.04g of the target compound, a white solid powder, melting point: 115-117°C; 1 H-NMR (CDCl 3 -d 6 ,500MHz)δ:7.92-7.88(d,1H),7.78-7.76(s,1H),7.53-7.49(d,1H),7.48-7.43(m,1H),7.32-7.28(m,1H), 5.07-5.04(s,2H),4.05-4.03(t,2H),3.84-3.80(s,3H),2.72-2.68(t,2H),2.04-1.99(m,2H),1.87-1.84(m ,2H).
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