Magnetic complex and preparation method thereof
A complex and magnetic technology, applied in the field of magnetic complexes and preparation thereof, achieves the effects of easy operation of the preparation method, short synthesis time and low cost
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Embodiment 1
[0025] Prepare 100mL of ethanol-water mixed solvent (ratio 3:2) and add it to the three-necked flask, weigh about 5g of solid NH 4 Cl and 9g of 2,3-dimethyl-2,3-dinitrobutane were added into a three-necked flask, and reacted at -10°C for 20min. Slowly add 20g of Zn powder into the three-necked flask within 2h, slowly rise to room temperature, react for 3h, then filter and dry to obtain 7g of 2,3-dimethyl-2,3-dihydroxyaminobutane. Weigh 4.4g of 2,3-dimethyl-2,3-dihydroxyaminobutane and dissolve it completely with 20mL of methanol, then add 5g of 2-indole formaldehyde, react at room temperature for 16-24h, and filter to obtain 6g of nitroxide free radical precursor. Dissolve 6 g of organic nitrogen oxide radical precursor in 20 mL of dichloromethane, add 48 g of lead oxide, stir at room temperature for 3 hours, and obtain 4.3 g of organic nitrogen oxide radical by column chromatography. 2.6gSm(hfac) 3 Mix with 100mL of n-hexane, heat to 80°C, reflux for 30min to dissolve the ...
Embodiment 2
[0027] Prepare 100mL of ethanol-water mixed solvent (ratio 3:2) and add it to the three-necked flask, weigh about 5g of solid NH 4 Cl and 9g of 2,3-dimethyl-2,3-dinitrobutane were added into a three-necked flask, and reacted at -10°C for 20min. Slowly add 20g of Zn powder into the three-necked flask within 2h, slowly rise to room temperature, react for 3h, then filter and dry to obtain 7g of 2,3-dimethyl-2,3-dihydroxyaminobutane. Weigh 4.4g of 2,3-dimethyl-2,3-dihydroxyaminobutane and dissolve it completely with 20mL of methanol, then add 5g of 2-indole formaldehyde, react at room temperature for 16-24h, and filter to obtain 6g of nitroxide free radical precursor. Dissolve 6 g of organic nitrogen oxide radical precursor in 20 mL of dichloromethane, add 48 g of lead oxide, stir at room temperature for 3 hours, and obtain 4.3 g of organic nitrogen oxide radical by column chromatography. 2.6gSm(hfac) 3 Mix with 100mL n-hexane, heat to 100°C, reflux for 30min to dissolve the sa...
Embodiment 3
[0029] Prepare 100mL of ethanol-water mixed solvent (ratio 3:2) and add it to the three-necked flask, weigh about 5g of solid NH 4 Cl and 9g of 2,3-dimethyl-2,3-dinitrobutane were added into a three-necked flask, and reacted at -10°C for 20min. Slowly add 20g of Zn powder into the three-necked flask within 2h, slowly rise to room temperature, react for 3h, then filter and dry to obtain 7g of 2,3-dimethyl-2,3-dihydroxyaminobutane. Weigh 4.4g of 2,3-dimethyl-2,3-dihydroxyaminobutane and dissolve it completely with 20mL of methanol, then add 5g of 2-indole formaldehyde, react at room temperature for 16-24h, and filter to obtain 6g of nitroxide free radical precursor. Dissolve 6 g of organic nitrogen oxide radical precursor in 20 mL of dichloromethane, add 48 g of lead oxide, stir at room temperature for 3 hours, and obtain 4.3 g of organic nitrogen oxide radical by column chromatography. 2.6gSm(hfac) 3 Mix with 100mL n-hexane, heat to 120°C, reflux for 30min to dissolve the sa...
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