chapter 2 palladium catalysts in suzuki cross- coupling reaction
chapter 2 palladium catalysts in suzuki cross- coupling reaction
chapter 2 palladium catalysts in suzuki cross- coupling reaction
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temperature, the catalyst was recovered by filter<strong>in</strong>g through a membrane filter with 0.2<br />
μm porosity and washed with ethyl acetate.<br />
Figure 4.2. The experimental set-up for Suzuki coupl<strong>in</strong>g <strong>reaction</strong>s<br />
4.3. Characterization of Products<br />
4.3.1. GC Method<br />
The samples were analyzed by GC/MS (HP GC/MS 6890/5973N on a HP-5MS,<br />
30m, 0.25 mm capillary column, 5% phenylmethoxysiloxane with 0.25μm film<br />
thickness) and GC (19091J-413 HP-5 6890N on a 30m, 0.25 mm capillary column (5%<br />
Dimetylsiloxane, 95% phenyldimethylsiloxane with a 0.25 μm film thickness and FID<br />
detector).<br />
The GC program applied throughout the analysis is as follows: the column<br />
temperature was 40 °C at the beg<strong>in</strong>n<strong>in</strong>g of the program and it was heated with a rate of<br />
10 °C/m<strong>in</strong> up to 250 °C, then it was kept at this temperature for 3 m<strong>in</strong>. Throughout the<br />
analysis the <strong>in</strong>jector and detector temperatures were kept constant at 280 °C and 300 °C,<br />
respectively. The analysis was performed on split mode with a split ratio of 1/50. A<br />
sample gas chromatogram of the reactant and <strong>reaction</strong> products accord<strong>in</strong>g to this<br />
temperature program is given <strong>in</strong> Figure 4.3.<br />
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