Method for synthesizing amine and imine
A synthesis method and compound technology, applied in chemical instruments and methods, preparation of organic compounds, condensation/addition reaction to prepare amino compounds, etc., can solve problems such as reaching 22.3%
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Embodiment 1
[0026] Weigh 0.0354gPdCl 2 , add 30 mL of deionized water to dissolve, add 2 mol / L hydrochloric acid to adjust the pH of the solution to 3, add 1 g of hydrotalcite HT to the above solution, stir at room temperature for 4 hours, and let stand for 10 hours. The mixture was evaporated to dryness at 45°C. The obtained powder was ground and dried at 120° C. for 10 hours to obtain a 2 wt % Pd / HT catalyst (Pd loading 0.2 mmol / g).
[0027] Catalyst performance evaluation was carried out in an atmospheric continuous reactor. Weigh 0.1g of 2wt% Pd / HT catalyst and add it into a 30mL reaction tube, add the reaction substrate benzyl alcohol 3mmol, nitrobenzene 1mmol, solvent toluene 2mL and internal standard n-dodecane 10μL under anaerobic conditions. The reaction temperature is controlled at 130 degrees Celsius by an oil bath. The above-mentioned reaction tube was placed in an oil bath with a stable temperature, and the reaction system was magnetically stirred at the same time, and the...
Embodiment 2
[0033] Weigh 0.0354gPdCl 2 , add 30 mL of deionized water to dissolve, add 2 mol / L hydrochloric acid to adjust the pH of the solution to 3, add 1 g of hydrotalcite HT to the above solution, stir at room temperature for 4 hours, and let stand for 10 hours. The mixture was evaporated to dryness at 45°C. The obtained powder was ground and dried at 120° C. for 10 hours to obtain a 2 wt % Pd / HT catalyst (Pd loading 0.2 mmol / g).
[0034] Catalyst performance evaluation was carried out in an atmospheric continuous reactor. Weigh 0.1g of 2wt% Pd / HT catalyst into a 30mL reaction tube, add 4mmol of benzyl alcohol, 1mmol of nitrobenzene, 2mL of solvent toluene and 10μL of internal standard n-dodecane under anaerobic conditions. The reaction temperature is controlled at 120 degrees centigrade by an oil bath. The above-mentioned reaction tube was placed in an oil bath with a stable temperature, and the reaction system was magnetically stirred at the same time, and the reaction timing st...
Embodiment 3
[0039] Weigh 0.0354gPdCl 2, add 30mL deionized water to dissolve, add 2mol / L hydrochloric acid to adjust the pH of the solution to 3, add 1g hydrotalcite HT to the above solution, stir at room temperature for 4 hours, and let stand for 10 hours. The mixture was evaporated to dryness at 45°C. The obtained powder was ground and dried at 120° C. for 10 hours to obtain a 2 wt % Pd / HT catalyst (Pd loading 0.2 mmol / g).
[0040] Catalyst performance evaluation was carried out in an atmospheric continuous reactor. Weigh 0.1g of 2wt% Pd / HT catalyst and add it into a 30mL reaction tube, add 15mmol of benzyl alcohol, 1mmol of nitrobenzene, solvent toluene and 10μL of internal standard n-dodecane under anaerobic conditions. The reaction temperature is controlled at 130 degrees Celsius by an oil bath. The above-mentioned reaction tube was placed in an oil bath with a stable temperature, and the reaction system was magnetically stirred at the same time, and the reaction timing started. ...
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