sodium iodide; acetonitrile;
reactants are commercially availlable.
ollis, kristin p., us2003/45546, a1, (2003) a) 5-chloro-2-iodo-pyridine to a refluxing solution of 2,5-dichloro-pyridine (12.2 g, 82.2 mmol), sodium iodide (37.0 g, 247 mmol) and acetonitrile (170 ml) under argon was added acetyl chloride (9. 0 ml, 127 mmol) and the solution was refluxed for 5 h. to the solution was added more sodium iodide (24.9 g, 166 mmol) and the solution was refluxed for 16 h. more sodium iodide (12.5 g, 83.6 mmol) wa s added and the solution was refluxed for 4.5 h. the solution was cooled to room temperature, and was partitioned between 10percent sodium thiosulfate/10percent aqueous sodium carbonate (300 ml) and e ther (400 ml). the ether layer was washed with brine (100 ml) and dried over anhydrous sodium sulfate. the solution was decanted, and dried in vacuo to yield 16.8 g (85percent) of the title compound a s a brown solid. 1h nmr (cdcl3): 8.36 (d, j=2.75 hz, 1h), 7.66 (d, j=8.79 hz, 1h), 7.32 (dd, j=8.38, 2.61 hz, 1h). there is 5 mol percent of starting material 2,5-dichloro-pyridine in the product as d etermined by nmr.
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