Preparation method of fullerene-polyoxometalate hybrid molecule
A polyoxometalate, fullerene technology, applied in the direction of organic chemistry, can solve the problem of difficult chemical modification, and achieve the effect of strong designability, novel structure and strong functionality
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Embodiment 1
[0041] (1) Take 9.87 mmol p-hydroxybenzaldehyde, 14.88 mmol anhydrous K 2 CO 3 In a 100 ml two-necked bottle, vacuumize and vent argon, repeat three times, inject N,N-dimethylformamide solution (40 ml) containing 12.84 mmoles of bromoacetate tert-butyl therein, 70 o C overnight. Filter to remove potassium carbonate, concentrate, transfer the concentrated solution to a separatory funnel, extract three times with ethyl acetate, combine the organic phases, dry over anhydrous magnesium sulfate, filter with suction, take the filtrate, and remove the organic solvent under reduced pressure. Dissolve the crude product in a small amount of n-hexane / ethyl acetate mixed solvent (the volume ratio of ethyl acetate is 30%), and use this as eluent for silica gel column chromatography to obtain tert-butyl acetate substituted Benzaldehyde. Pale yellow solid with a yield of 70.39%.
[0042] (2) Add 2.54 mmol C 60 and 8.50 mmoles of sarcosine, vacuumize, and flow argon, repeat three times, ...
Embodiment 2
[0056] On the basis of Example 1, the p-hydroxybenzaldehyde in step (1) was replaced by 2,4-dihydroxybenzaldehyde, the amount of tert-butyl bromoacetate was adjusted to 25.68 mmol, anhydrous K 2 CO 3 The amount of addition is adjusted to 20 mmoles; Dawson-NH in step 4 2 The addition amount of is adjusted to 0.80 mmol, and other conditions are unchanged.
Embodiment 3
[0058] On the basis of Example 2, p-hydroxybenzaldehyde in step (1) was replaced by 2,5-dihydroxybenzaldehyde, and other conditions remained unchanged.
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