C60 derivative containing cyclic phenyl imine ester structure and method for preparing the same
A technology of cyclophenyl imide esters and derivatives, applied in the field of fullerene derivatives
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Embodiment 16
[0028] Example 1 [6,6] Cyclophenylimidate C 60 preparation of
[0029] In 100mL of 0.05M tetrabutylammonium perchlorate in benzonitrile solution, add 200mg C 60 , at N 2Under the protection of , the saturated calomel electrode was used as the reference electrode, and the reduction potential of -1.6V was applied to carry out the controlled potential bulk electrolysis. Check the cyclic voltammetry of the solution until an irreversible oxidation peak appears at -0.51V (eg figure 1) , to stop the electrolytic reduction. Adjust the potential to 0V, and carry out oxidation electrolysis to complete. The solvent was removed by rotary evaporation, washed with methanol to remove tetrabutylammonium perchlorate, filtered, and dried in a vacuum oven to give [6,6]cyclophenylimidate C 60 crude product. Taking Buckyprep as the separation, using toluene as mobile phase, separating and purifying by high-performance liquid chromatography, and finally obtaining pure [6,6] cyclophenylimidate...
Embodiment 2
[0030] Example 2 [6,6] Cyclophenylimidate C 60 preparation of
[0031] A benzonitrile solution of 0.5M tetrabutylammonium perchlorate was used for the reaction, the applied potential was -1.0V, and the rest of the operations were as in Example 1.
Embodiment 3
[0032] Example 3 [6,6] Cyclophenylimidate C 60 preparation of
[0033] A 0.2M tetrabutylammonium perchlorate solution in benzonitrile was used for the reaction, the applied potential was -1.2V, and the rest of the operations were as in Example 1.
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