1,4- dihydropyridine ring-containing cis-nitenpyram compound, preparation method and application thereof
A dihydropyridine ring cis-nitenpyram and compound technology, which is applied in the field of cis-nitenpyram compounds and their preparation, can solve problems such as poor hydrophobicity and light instability, achieve low toxicity, and use methods Simplicity and significant practical effect
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Embodiment 1
[0042] cis-1-methyl-4-phenyl-3-ethoxycarbonyl-2-amino-6-[N-(6'-chloro-3'-pyridylmethyl)-N-ethyl]amino-5- Nitro-1,4-dihydropyridine (Ia);
[0043] Dissolve benzaldehyde (1.06g, 10mmol) in absolute ethanol (30mL) at room temperature, add ethyl cyanoacetate (1.4ml, 10mmol), add dropwise 0.5ml of piperidine and stir at room temperature for 2 hours, then add The compound nitenpyram (10mmol, 2.707g) was heated to reflux, and the reaction was tracked by TLC. After the reaction was completed, it was cooled, and the solvent was distilled off under reduced pressure, dissolved in 10mL of water and extracted three times with 60mL of ethyl acetate. The combined extracts were dried overnight with anhydrous magnesium sulfate, and the solvent was distilled off to obtain a yellow oil. Column chromatography with ethyl acetate:petroleum ether=2:1 gave a yellow solid with a yield of 81.23%.
[0044] Elemental Analysis: Calculated C% 58.53 H% 5.55 N% 14.84
[0045] Measured value C% 58.12 H% 6....
Embodiment 2
[0050] Preparation of cis-1-methyl-4-(4'-bromophenyl)-3-ethoxycarbonyl-2-amino-6-[N-(6'-chloro-3'-pyridylmethyl)-N- Ethyl]amino-5-nitro-1,4-dihydropyridine (Ib);
[0051] Dissolve p-bromobenzaldehyde (1.83g, 10mmol) in absolute ethanol (30mL) at room temperature, add ethyl cyanoacetate (1.4ml, 10mmol), dropwise add 0.5ml of piperidine and stir at room temperature for 2 hours, Then the compound nitenpyram (10mmol, 2.707g) was added and heated to reflux, and the reaction was tracked by TLC. After the reaction was completed, it was cooled, and the solvent was distilled off under reduced pressure, dissolved in 10mL of water and extracted three times with 60mL of ethyl acetate. The combined extracts were dried overnight with anhydrous magnesium sulfate, and the solvent was distilled off to obtain a yellow oil. Column chromatography with ethyl acetate:petroleum ether=2:1 gave a yellow solid with a yield of 51.73%.
[0052] Elemental analysis: found value C% 50.18 H% 4.54 N% 12.74 ...
Embodiment 3
[0058] Preparation of cis-1-methyl-4(-2'-chlorophenyl)-3-ethoxycarbonyl-2-amino-6-[N-(6'-chloro-3'-pyridylmethyl)-N- Ethyl]amino-5-nitro-1,4-dihydropyridine (Ic);
[0059] Dissolve 2-chlorobenzaldehyde (1.41g, 10mmol) in absolute ethanol (30mL) at room temperature, add ethyl cyanoacetate (1.4ml, 10mmol), add dropwise 0.5ml of piperidine and stir at room temperature for 2 hours , then add the compound nitenpyram (10mmol, 2.707g) and heat to reflux, TLC tracking reaction, after the reaction is cooled, evaporate the solvent under reduced pressure, add 10mL water to dissolve and extract three times with 60mL ethyl acetate. The combined extracts were dried overnight with anhydrous magnesium sulfate, and the solvent was distilled off to obtain a yellow oil. Column chromatography with ethyl acetate:petroleum ether=2:1 gave a yellow solid with a yield of 65.49%.
[0060] Elemental Analysis: Calculated C% 54.55 H% 4.98 N% 13.83
[0061] Found value C% 54.49 H% 4.98 N% 13.96
[0062...
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