A kind of abamectin b2a/b2b derivative substituted by sulfonamide group and its preparation method and application
A technology based on abamectin and sulfonamide group, which is applied in the preparation of sugar derivatives, botanical equipment and methods, sugar derivatives, etc., and can solve problems such as poor stability of chemical properties, resistance of pests, and poor control effects , to achieve the effects of not easy to decompose and inactivate, high insecticidal activity, and improved control effect
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Embodiment 1
[0069] 4"-Deoxy-4"-N,N-p-toluenesulfonylmethylaminoabamectin B 2a / B 2b The preparation method:
[0070] 10g 5-allyloxycarbonyl-4"-N-methylaminoabamectin B 2a / B 2b (Content >90%) dissolved in 40ml of sec-butyl acetate, after heating up to 60°C, add 1.8g of p-toluenesulfonyl chloride dropwise, 2.0g of tetramethylethylenediamine and keep warm for 0.5h; cool down to -10°C, add 2g Methanol, 1.3g sodium borohydride, 0.005g Pd(PPH 3 ) 2 Cl 2 React for 0.5h; then add 7.6% phosphoric acid solution to adjust the pH to 2, and then use 10% sodium hydroxide solution to adjust the pH to 7. After standing and layering, the organic phase is dried with anhydrous sodium sulfate, and concentrated after removing the inert solvent under reduced pressure The residue was purified by column chromatography to obtain a light yellow solid (content>90%).
[0071] Compound 4"-deoxy-4"-N,N-p-toluenesulfonamidomethylaminoabamectin B 2a / B 2b The structural identification data for:
[0072] l HN...
Embodiment 2
[0076] 4"-Deoxy-4"-N,N-cyclopropanesulfonamidomethylaminoabamectin B 2a / B 2bThe preparation method:
[0077] 10g compound 5-allyloxycarbonyl-4"-N-methylaminoabamectin B 2a / B 2b (Content >90%) was dissolved in 30g of dichloromethane (solvent), 1.9g of cyclopropanesulfonyl chloride and 2.0g of triethylamine were added dropwise at -10°C, and the reaction was kept for 2 hours. After the reaction of the raw materials was completed, the temperature was lowered to -20°C, and 1.5 g of methanol, 1.0 g of sodium borohydride and 0.003 g of palladium acetate were added to react for 2 h. Add 7.6% phosphoric acid solution to adjust the pH to 2.5, and then use 10% sodium hydroxide solution to adjust the pH to 7.5. After standing and stratifying, the organic phase is dried with anhydrous sodium sulfate, and the inert solvent is removed under reduced pressure. After purification by column chromatography, a light yellow solid (content >90%) was obtained.
[0078] Compound 4"-deoxy-4"-N,N...
Embodiment 3
[0083] 4"-Deoxy-4"-N,N-(4-pyridine)sulfonamidoaminoabamectin B 2a / B 2b The preparation method:
[0084] 10g compound 5-allyloxycarbonyl-4"-N-methylaminoabamectin B 2a / B 2b (Content>90%) was dissolved in 40ml of dimethylformamide, and after heating up to 50°C, 2.9g of pyridine-4-sulfonyl chloride and 2.0g of pyridine were added dropwise, and the reaction was kept for 1h. Cool down to 0°C, add 4g of methanol, 1.5g of sodium borohydride, and 0.008g of palladium chloride to react for 1 hour. Add 10% phosphoric acid solution to adjust the pH to 1.5, and then use 15% sodium hydroxide solution to adjust the pH to 6.5. After standing and stratifying, the organic phase is dried with anhydrous sodium sulfate, and the inert solvent is removed under reduced pressure. After purification by column chromatography, a light yellow solid (content >90%) was obtained.
[0085] LC-MS[M+H] + : 1045.5301. 4"-Deoxy-4"-N,N-(4-pyridine)sulfonamidomethylaminoabamectin B 2a [M+H] of + Calculate...
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