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Aryl triflates were prepared from the corresponding phenols by a well-established method: Echavarren, A. M.; Stille, J. K. J. Am. Chem. Soc. 1987, 109, 5478.
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Aryl triflates were prepared from the corresponding phenols by a well-established method: Echavarren, A. M.; Stille, J. K. J. Am. Chem. Soc. 1987, 109, 5478.
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A 50 mL round-bottom flask was charged with 4-methoxyphenol (1.86 g, 15 mmol) and sealed with a septum. Subsequently, pyridine (15 mL) was added. The clear solution was cooled to 0°C and trifluoromethanesulfonic anhydride (2.8 mL, 17 mmol) was added dropwise. The resulting orange solution was stirred over night at r.t. Another 10 mL Schlenk flask was charged with Pd(OAc)2 (50.5 mg, 1.5 mol, 1,3-bis(diphenylphosphino)propane (139.2 mg, 2.25 mol, DMF (5 mL, and 2-butoxyethyl ether (2.61 mL, internal GC standard, Both solutions were combined and transferred to a 100 mL autoclave of the 4560 series from Parr Instruments® under argon atmosphere. After flushing the autoclave three times with CO/H2 1:1, 20 bar of synthesis gas were adjusted at ambient temperature and the reaction was performed for 24 h at 100°C. Before and after the reductive carbonylation an aliquot of the reaction mixture was subjected to GC analysis for determination of yield and c
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2 (1:1), 20 bar of synthesis gas were adjusted at ambient temperature and the reaction was performed for 24 h at 100°C. Before and after the reductive carbonylation an aliquot of the reaction mixture was subjected to GC analysis for determination of yield and conversion.
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