A kind of diazoamide hydrazone pyridine derivative and its synthesis method and application
A diazamide hydrazone pyridine and synthesis method technology, which is applied in the field of synthesis of new compounds, can solve problems such as the complexity of the B component of the extractant solution, and achieve the effects of strong extraction capacity, mild reaction conditions, and high extraction efficiency
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Embodiment 1
[0052] (1) Add 1.27g of aminehydrazone pyridine (2) and 5.0ml of triethylamine into 250.0ml of ethanol, and stir in a 500.0mL three-neck flask; dissolve 2.4g of camphorquinone (1) in 50.0mL of ethanol, and The constant pressure funnel was added dropwise into the above-mentioned three-neck flask, and the dropwise reaction was carried out for 30 minutes, and then stirred and refluxed for 7 days under the protection of nitrogen.
[0053] The progress of the reaction was followed by TLC (Thin Layer Chromatography) and the reaction time was adjusted.
[0054] (2) After stopping the reaction, the mixed solution was cooled to room temperature, filtered through a sand core funnel to remove solid impurities, and the filtrate was evaporated to obtain an oily substance; the oily substance was dissolved with dichloromethane, and petroleum ether / ethyl acetate (volume ratio 1 / 3) As a developer, the dichloromethane mixture of the oil was purified by silica gel column chromatography to obtai...
Embodiment 2
[0060] (1) Add 1.27g aminehydrazone pyridine (compound 2) and 5.0ml triethylamine to 250.0ml tetrahydrofuran solvent and stir in a 500.0mL three-neck flask; dissolve 2.4g camphorquinone (compound 1) in 50.0mL ethanol In the above-mentioned three-necked flask through a constant pressure funnel, the dropwise reaction was carried out for 30 minutes, and then stirred and refluxed for 7 days under the protection of nitrogen.
[0061] The reaction was followed by TLC (Thin Layer Chromatography).
[0062] (2) After stopping the reaction, the mixed solution was cooled to room temperature, filtered through a sand core funnel to remove solid impurities, and the filtrate was evaporated to obtain an oily substance; the oily substance was dissolved with dichloromethane, and petroleum ether / ethyl acetate (volume ratio 1 / 3) As a developer, the dichloromethane solution of the oily substance was purified by silica gel column chromatography to obtain a crude product, which was then recrystalli...
Embodiment 3
[0064] (1) Add 3.0 g of amide hydrazone pyridine (compound 2) and 8 ml of triethylamine into 450.0 ml of ethanol solvent, and stir in a 500.0 mL three-neck flask; dissolve 6.0 g of camphorquinone (compound 1) in 50.0 mL of ethanol, Add it dropwise into the above-mentioned three-neck flask through a constant pressure funnel, perform dropwise reaction for 30 minutes, and then stir and reflux for 10 days.
[0065] The reaction was followed by TLC (Thin Layer Chromatography).
[0066] (2) After stopping the reaction, the mixed solution was cooled to room temperature, filtered through a sand core funnel to remove solid impurities, and the filtrate was evaporated to obtain an oily substance; the oily substance was dissolved with dichloromethane, and petroleum ether / ethyl acetate (volume ratio 1 / 3) As a developer, the dichloromethane solution of the oily substance was purified by silica gel column chromatography to obtain a crude product, which was then recrystallized with ethanol a...
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