Agilent 7890a gc 5973 ms

In a typical experiment, the desired substrates, catalyst, and solvent were charged into an autoclave (50 mL inner volume). After the reactor was sealed, it was purged with 5 atm. O₂. Then, the reactor was put into a constant temperature air bath at the desired temperature, and the magnetic stirrer was started. After a certain reaction time, the reactor was placed into ice water, and then the gases in the reactor were released slowly and 0.5 mmol ethylbenzene as internal standard was added into the reactor followed by filtration. The reaction mixture was then analyzed quantitatively by GC (Agilent 7820A) equipped with a flame-ionized detector, and the products were confirmed by GC-MS (Agilent 7890A GC/5973 MS). To obtain the pure products, the reaction mixture was concentrated and purified by column chromatography (silica gel with n-hexane/EtOAc). The pure products were characterized by ¹H NMR and ¹³C NMR. To examine the reusability of the Zn/NC-950, the catalyst was recovered by centrifugation, washed with methanol, and calcined at 400 °C under N₂ for 2 h. Then the catalyst was used for the next run.

In a typical hydrogenation reaction, nitroaromatic (0.25 mmol), catalyst (36 mg, Ru 0.77 mol%, Pd 1.01 mol%) and ethanol (2.0 mL) were added to a Teflon-lined steel autoclave. Before reaction, the autoclave was sealed and flushed with H₂ three times to remove the air. Then the autoclave was charged with a 2.0 MPa H₂ at room temperature, and then heated from room temperature to 80 °C within 20 min and kept at this temperature under magnetic stirring (900 rpm). After the completion of the reaction, the autoclave was cooled down to room temperature. The products were analyzed by a gas chromatograph (Agilent 7890 A) equipped with an HP-5 column, and further confirmed by GC–MS (Agilent 7890 A GC/5973 MS). After each run the catalyst was separated from the reaction mixture by centrifugation, thoroughly washed with ethanol for five times, and dried at 60 °C under a vacuum for the next reaction cycle. After the sixth reaction cycle, the catalyst was recovered by centrifugation for characterization and the residual filtrate was allowed for further reaction under the same conditions. All of the error bars represent the standard deviations from three repeated experiments.