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Passing the chloromethylpicolinate 10 through a charcoal filter allowed the reaction to reach completion after the first [Pd]/ligand charge. We chose not to scale this option for our pilot-plant campaign.
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As the completed reaction was cooled from the set point of 180 °C, it tended to set to a hard, glasslike material at 165 °C. Addition of a high boiling solvent (such as 1,2 dichlorobenzene) to mobilise the melt was demonstrated, but this overall workup was still judged to be risky (albeit after minimal development).
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As the completed reaction was cooled from the set point of 180 °C, it tended to set to a hard, glasslike material at 165 °C. Addition of a high boiling solvent (such as 1,2 dichlorobenzene) to mobilise the melt was demonstrated, but this overall workup was still judged to be risky (albeit after minimal development).
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