A kind of preparation method and application of 3-methoxy-4-(5-bromopentyloxy) phenylfullerene pyrrolidine
A technology of fullerene pyrrolidine and bromopentyloxy, which is applied in chemical instruments and methods, hydrogenation hydrocarbon production, catalyst supports, etc., and can solve undisclosed fullerene pyrrolidine and undisclosed fullerene pyrrolidine preparation methods And other issues
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Embodiment 1
[0070] The synthetic method of N-methyl-2-[3-methoxy-4-(5-bromopentyloxy) phenyl]-3,4-fullerene pyrrolidine comprises the following steps:
[0071] (1) Synthesis of 3-methoxy-4-(5-bromopentyloxy)benzaldehyde
[0072] According to nucleophilic substitution reaction, in 250mL three-neck flask, add 760mg (5mmol) 3-methoxy-4-hydroxybenzaldehyde and make it dissolve in 180mL acetone, then add excess potassium carbonate (K 2 CO 3 ), heated and stirred for about 30 minutes under the protection of argon (Ar) to dissolve completely, then added excess 1,5-dibromopentane, heated to reflux for 8 hours, cooled and filtered to obtain a slightly yellow solution, which was separated by chromatographic column product, with V 石油醚 :V 乙酸乙酯 =5:1 is the eluting product of the developer, and the product solution was evaporated by rotary evaporation to obtain a light yellow viscous liquid, which became a powdery solid after vacuum drying for 24 hours, with a yield of 91.0%.
[0073] The product was...
Embodiment 2
[0082] Thermal stability of N-methyl-2-[3-methoxy-4-(5-bromopentyloxy)phenyl]-3,4-fullerene pyrrolidine
[0083] The thermal stability of the product in air atmosphere was studied by DTA-60 microcomputer differential calorimeter. The temperature rise rate of the alumina pool is 10°C / min, and the test temperature range is from room temperature to 600°C. The thermogravimetric analysis is as follows: figure 2 shown;
[0084] by attaching figure 2 It can be seen that the product decomposes after being heated, showing exothermic decomposition, and the peak temperature of the decomposition exothermic peak is 444.04°C. It can be considered that the product has good thermal stability and is a further derivation of a single-addition derivative at a higher temperature. transformation offers the possibility.
Embodiment 3
[0086] N-methyl-2-[3-methoxy-4-(5-bromopentyloxy)phenyl]-3,4-fullerene pyrrolidine is used as a catalyst carrier, and its specific steps are as follows:
[0087] Preparation of Pd-supported N-methyl-2-[3-methoxy-4-(5-bromopentyloxy)phenyl]-3,4-fullerene pyrrolidine nanoparticle catalyst
[0088] (1) Weigh 100mg N-methyl-2-[3-methoxy-4-(5-bromopentyloxy)phenyl]-3,4-fullerene pyrrolidine and place it in a round bottom flask, Add 100mL deionized water, sonicate for 4h to make N-methyl-2-[3-methoxy-4-(5-bromopentyloxy)phenyl]-3,4-fullerenepyrrolidine evenly dispersed in deionized water;
[0089] (2) Weigh 20 mg of sodium chloropalladate and dissolve it in 10 mL of deionized water to dissolve it completely, add it to the above-mentioned round bottom flask, and place it in an oil bath at 85°C with magnetic stirring to make N-methyl-2-[3 -Methoxy-4-(5-bromopentyloxy)phenyl]-3,4-fullerene pyrrolidine and Na 2 PdCl 4 mix evenly;
[0090] (3) Add 2 mL of 1.0 mmol / L NaBH to the new ...
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