Preparation method and application of a supported cnts@nhc-cu catalytic material
A catalytic material and supported technology, applied in the field of catalysis, to achieve the effect of mild reaction conditions and simple process
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[0050] A preparation method of supported CNTs@NHC-Cu catalytic material, comprising the following steps:
[0051] ⑴Preparation of 2-(2-bromoethoxy)pyrene (2-(2-bromoethoxy)pyrene):
[0052] To a 100 mL round bottom flask was added 1-hydroxypyrene (2.18 g, 10 mmol), Cs 2 CO 3 (6.5 g, 20 mmol), 1,2-dibromoethane (7.48 g, 40 mmol) and acetonitrile (35 mL), stirred under reflux at 60~80°C for 24 h. After the reaction was completed, cool to room temperature to obtain reaction solution A; add water (50 mL) to reaction solution A, and extract the resulting solution with dichloromethane (3×30 mL), dry dichloromethane with anhydrous magnesium sulfate solution, filtered, and rotovaped to remove solvent. The obtained product was purified by column chromatography (ethyl acetate:petroleum ether=1:4) to obtain a yellow solid substance: 2-(2-bromoethoxy)pyrene with a yield of 70%.
[0053] ⑵Preparation of 1-(2-(pyren-2-oxy)ethyl)-1H benzo[d]imidazole (1-(2-(pyren-2-yloxy)ethyl)-1H-benzo[...
Embodiment 1
[0073] In a Schlenk glass reaction vial with a screw cap, add 1.0 mmol benzyl azide, 1.2 mmol phenylacetylene and 1 mol% NHC-Cu molecular catalyst (relative to benzyl azide). The reaction was stirred for 3 hours under the condition of no solvent and the reaction temperature was 30° C., and then the product was dissolved, filtered, and the solvent was removed by rotary evaporation. The obtained crude product was washed several times with n-hexane and water to remove unreacted substrate, and then dried at 60°C to obtain the target product 1-benzyl-4-phenyl-1,2,3-triazole (1-benzyl -4-phenyl- 1H -1,2,3-triazole), the separation yield was 93%, and the purity of the product was over 95% as determined by NMR.
[0074] The NMR data of the product are as follows:
[0075] 1 H NMR (CDCl 3 , 400 MHz) δ (ppm): 5.53 (s,2H), 7.26–7.41 (m, 6H), 7.69(s, 1H), 7.79–7.82 (m, 4H)
[0076] 13 C NMR (CDCl 3 , 101 MHz) δ (ppm): 54.1, 119.7, 125.7, 128.0, 128.2,128.7, 128.8, 129.1, 130.6, 134...
Embodiment 2
[0078] In a Schlenk glass reaction vial with a screw cap, add 1.0 mmol benzyl azide, 1.2 mmol phenylacetylene and 1 mol% NHC-Cu molecular catalyst (relative to benzyl azide), using 3 mL methanol as solvent, The reaction was stirred for 3 hours at a reaction temperature of 30° C., and then the product was dissolved, filtered, and the solvent was removed by rotary evaporation. The obtained crude product was washed several times with n-hexane and water to remove the unreacted substrate, and then dried at 60°C to obtain the target product 1-benzyl-4-phenyl-1,2,3-triazole, and the isolated yield was 66%, and the purity of the product is over 95% as determined by NMR.
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