Synthetic method of N-benzylideneaniline compound
A technology for benzylidene aniline and compound is applied in the field of synthesizing N-benzylidene aniline compounds, and achieves the effects of low cost, environmental friendliness, high activity and stability
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Embodiment 1
[0037] 1) Preparation of porous carbon carrier, 9.4g of phenol at 50°C, add 10mL of 0.5mol / L sodium hydroxide solution, stir for 10-15 minutes, add dropwise 4.1g of 37% formaldehyde solution, phenol, formaldehyde and sodium hydroxide The molar ratio is 2:1:0.1, the temperature rises to 85-95°C, reacts under stirring for 1 hour, the temperature drops to room temperature, adjusts the pH value to neutrality with 0.5mol / L hydrochloric acid solution, and then removes the water by vacuum distillation to obtain Brown liquid 11g, add absolute ethanol to prepare 20% phenolic resin absolute ethanol solution. Dissolve 8g of F127 in 32g of absolute ethanol, the mass ratio of which is 1:4, mix with the above-mentioned 20% phenolic resin absolute ethanol solution, let stand at room temperature for 4 to 6 hours, distill under reduced pressure to remove ethanol, and then Thermally polymerized at 100-120°C for 24 hours to obtain a polymer. Finally, in a tubular resistance furnace under nitroge...
Embodiment 2
[0041] The catalyst preparation process is the same as in Example 1, except that the palladium loading of the catalyst is 5.0%, that is, adding 1 g of porous carbon carrier to 5 mL of Pd with a mass concentration of 0.010 g / mL of H 2 PdCl 6 The solution was magnetically stirred at room temperature for 2 hours, then 0.073 g of sodium borohydride was added as a reducing agent, and the subsequent steps were the same to prepare a supported palladium catalyst with a palladium loading of 5%. 0.36 gram of catalyst was added into 100 milliliters of reactor, other reaction conditions were the same as in Example 1, and the reaction time was 16 hours. Gas chromatography detected that the conversion rate of nitrobenzene was 100%, and the selectivity of N-benzylidene aniline was 85.0%.
Embodiment 3
[0043] Catalyst preparation process is the same as embodiment 1, and difference is that catalyst palladium content is 3.0%, and the mass concentration that is about to add 1g porous carbon carrier to 3mL Pd is the H of 0.010g / mL. 2 PdCl 6 The solution was magnetically stirred at room temperature for 2 hours, then 0.044 g of sodium borohydride was added as a reducing agent, and the subsequent steps were the same to prepare a supported palladium catalyst with a palladium loading of 3%. 0.36 gram of catalyst was added into 100 milliliters of reactor, other reaction conditions were the same as in Example 1, the reaction time was 18 hours, the conversion rate of nitrobenzene was 100% as detected by gas chromatography, and the selectivity of N-benzylidene aniline was 97.8%.
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