A kind of preparation method of Schiff base vanadyl complex crystal with biological activity
A technology of Schiff base vanadyl and biological activity, which is applied in the direction of preparation of imino compounds, compounds of group 5/15 elements of the periodic table, drug combinations, etc. Small problems, to achieve good anti-diabetic activity, simple method, short time
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Embodiment 1
[0015] The first step is to dissolve 0.6532g of 3-chloropropylamine hydrochloride in 25ml of absolute ethanol solvent, add 0.53ml of salicylaldehyde, stir until dissolved, add 1ml of 5mol / L NaOH aqueous solution to the system, and reflux at 70°C for 3.5 hours Finally, 10 ml of methanol and 20 ml of chloroform were added to the system to obtain a yellow turbid mixture.
[0016] The second step is to filter the yellow turbid mixture obtained in the first step, add 10ml of methanol solution containing 0.6624g of vanadyl acetylacetonate to the filtrate, stir and reflux at 55°C for 3 hours and then filter, the filtrate is placed at room temperature for 8 days to precipitate yellow Green crystals.
[0017] The third step is to take out the crystals in the reaction vessel, wash them with methanol three times, then wash them with absolute ethanol and ether three times, place them in a desiccator, and obtain dry and pure crystals after 1 hour, that is, biologically active Schiff base o...
Embodiment 2
[0020] The first step is to dissolve 0.6530g of 3-chloropropylamine hydrochloride solid in 25ml of anhydrous methanol solvent, add 0.5ml of salicylaldehyde liquid, stir until dissolved, then add 1ml of 5mol / L NaOH aqueous solution to the system, 65℃ After reflux reaction for 4 hours, 10 ml of methanol and 20 ml of chloroform were added to the system to obtain a yellow turbid mixture.
[0021] The second step is to filter the yellow clear and transparent solution obtained in the first step, add 10ml of methanol solution containing 0.6665g of vanadyl acetylacetonate to the filtrate, stir and reflux at 60°C for 3 hours and then filter, and the filtrate is placed at room temperature for 9 days to precipitate Yellow-green crystals.
[0022] The third step is to take out the crystals at the bottom of the container, wash them with methanol three times, then wash them with absolute ethanol and ether three times respectively, place them in a desiccator, and obtain dry and pure crystals...
Embodiment 3
[0025] The first step is to dissolve 0.6553g of 3-chloropropylamine hydrochloride solid in 25ml of anhydrous methanol solvent, add 0.54ml of salicylaldehyde liquid, stir until dissolved, then add 1ml of 5mol / L NaOH aqueous solution to the system, 65℃ After reflux reaction for 4 hours, 10 ml of methanol and 20 ml of chloroform were added to the system to obtain a yellow turbid mixture.
[0026] The second step is to filter the yellow turbid mixture obtained in the first step, add 10ml of methanol solution containing 0.6674g of vanadyl acetylacetonate to the filtrate, stir and reflux at 58°C for 3 hours, then filter, and leave the filtrate at room temperature for 7 days to precipitate yellow Green rhombohedral crystals.
[0027] The third step is to take out the crystals in the reaction vessel, wash them with methanol three times, then wash them with absolute ethanol and ether three times, place them in a desiccator, and obtain dry and pure crystals after 1 hour, that is, biolog...
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