Process for the preparation of pesticide imidacloprid
A technology for preparing insecticides and imidacloprid, applied in botany equipment and methods, biocides, animal repellents, etc., can solve problems such as difficult operation and trouble, and achieve avoiding bumping, improving solubility, and high yield Effect
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Embodiment 1
[0018] Sodium hydroxide (6g) was added to a solution of 2-nitroiminoimidazolidine (16g, 0.123mol) in dimethylformamide (50ml). The temperature of the reaction mixture was lowered to 50°C with a water bath. To the reaction mixture was added a solution of 2-chloro-5-chloromethylpyridine (20 g, 0.123 mol) in dimethylformamide (100 ml) over 4 hours. Heating of the reaction mixture was continued at the same temperature for 4 hours. The reaction mixture was stirred well. After the reaction was complete, the reaction mixture was filtered. The residue contained sodium chloride (7g). The filtrate was concentrated by distillation under reduced pressure, and poured into distilled water (100 ml). The pH of the solution was adjusted to 4 with dilute hydrochloric acid to precipitate imidacloprid, which was filtered off and washed with methanol (90 ml). The yield was 23 g, the yield was 76.6%, and the purity was 94.16%.
Embodiment 2
[0020] Sodium hydroxide (6g) was added to a solution of 2-nitroiminoimidazolidine (18g, 0.138mol) in dimethylformamide (50ml). The temperature of the reaction mixture was lowered to 50°C with a water bath. To the reaction mixture was added a solution of 2-chloro-5-chloromethylpyridine (20 g, 0.123 mol) in dimethylformamide (100 ml) over 4 hours. Heating of the reaction mixture was continued at the same temperature for 4 hours. The reaction mixture was stirred well. After the reaction was complete, the reaction mixture was filtered. The residue contained sodium chloride (6.45g). The filtrate was concentrated by distillation under reduced pressure, and poured into distilled water (100 ml). The pH of the solution was adjusted to 4 with dilute hydrochloric acid to precipitate imidacloprid, which was filtered off and washed with methanol (90 ml) to yield 20 g, 66.6% yield and 95.18% purity.
Embodiment 3
[0022] Sodium hydroxide (3g) was added to a solution of 2-nitroiminoimidazolidine (18g, 0.138mol) in dimethylformamide (50ml). The temperature of the reaction mixture was lowered to 50°C with a water bath. To the reaction mixture was added a solution of 2-chloro-5-chloromethylpyridine (20 g, 0.123 mol) in dimethylformamide (100 ml) over 4 hours. After half of the 2-chloro-5-chloromethylpyridine solution was added to the reaction mixture, sodium hydroxide (3 g) was further added to the reaction mixture. Heating of the reaction mixture was continued at the same temperature for 4 hours. The reaction mixture was stirred well. After the reaction was complete, the reaction mixture was filtered. The residue contained sodium chloride (7.4g). The filtrate was concentrated by distillation under reduced pressure, and poured into distilled water (100 ml). The pH of the solution was adjusted to 4 with dilute hydrochloric acid to precipitate imidacloprid, which was filtered off and was...
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