7820a agilent gc system chromatograph

A mixture of iodobenzene (1 mmol), phenylacetylene (1.5 mmol), Et₃N (2 mmol), H₂O (1 cm³) and the catalyst (10 mg of G-(H₂L)-Pd) was stirred under aerobic conditions at a constant temperature (50 or 70 °C). The progress of the reaction was monitored by gas chromatography (GC). After completion, CHCl₃ (10 cm³) was added to the reaction mixture and the catalyst was recovered by filtration and washed with CHCl₃ (2 × 5 cm³) and H₂O (2 × 5 cm³). The organic layers were collected and dried over anhydrous Na₂SO₄. The analysis of the reaction products in the organic phase was performed by GC using a 7820A Agilent GC System chromatograph, with an Agilent 190915-433 column, 30 m × 250 µm × 25 µm and a flame ionization detector (FID) (Agilent, Santa Clara, CA, USA). The recovered catalyst was reused for another batch of the same reaction. The process was repeated for three additional runs.

A mixture
of iodobenzene (1 mmol), phenylacetylene (1.5 mmol), Et₃N (2 mmol), H₂O (1 cm³), and the catalysts
(from 15 to 25 mg), with reactants/Pd(II) = 100, was stirred under
aerobic conditions at a constant temperature (50 °C). The progress
of the reaction was monitored by gas chromatography (GC). After completion,
CHCl₃ (10 mL) was added to the reaction mixture and the
catalyst was recovered by filtration and washed with CHCl₃ and H₂O. The organic layers were collected and dried
over anhydrous Na₂SO₄. The analysis of the reaction
products in the organic phase was performed by GC using a 7820A Agilent
GC System chromatograph with an Agilent 190915-433 column (30 m ×
250 μm × 25 μm) and a flame ionization detector (FID).
A further check of the reaction products was carried out by random
sampling to analyze the composition of the reaction crudes by means
of ¹³C and ¹H NMR spectroscopy. For illustrative
purposes, some of the results obtained are shown in Figure S4 and Table S3. The corresponding NMR spectra were
obtained by using a 400 MHz NMR spectrometer (Bruker, AVANCE NEO 4400).
The procedure was as follow: the crude products were evaporated under
reduced pressure, and then 30 mg of each residue was dissolved in
0.5 mL of CDCl₃ and the NMR spectra were recorded. The
recovered catalysts were reused for three additional runs, repeating
the same procedure.