Ethanol → 3,6-Dibromopyridine-2-carbaldehyde

Temperatur

80 °C

A solution of silver nitrate (8.5 g, 50 mmol) in water (26 mL) was added dropwise to a solution of compound 84 (8.17 g, 20 mmol) in refluxing EtOH (100 mL). The mixture was stirred at 80° C. for 5 hours. After the mixture was cooled to room temperature, it was diluted with water (100 mL), extracted with EtOAc (3×), dried over Na2SO4, filtered and concentrated under reduced pressure. The product was obtained after silica gel chromatography eluting with 0-40% EtOAc in hexane (2.85 g, 51% over two steps).

1. temperatureAfter the mixture was cooled to room temperature
2. extractionextracted with EtOAc (3×)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe product was obtained after silica gel chromatography
7. washeluting with 0-40% EtOAc in hexane (2.85 g, 51% over two steps)

ORD-Eintrag

ord-770831a3eb274f6183db94c0cbf2fca2

Quelldatensatz

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08283358B2