3,5-Dibromopyridine → HCID 59777373, Verbindung

To a degassed solution of 3,5-dibromopyridine (0.4 g, 1.7 mmol), sodium tert-butoxide (227 mg, 3.6 mmol), tris(dibenzylideneacetone)dipalladium (145 mg, 0.09 mmol) and rac-BINAP (105 mg, 0.2 mmol) in dry toluene (10 mL) was added 1-phenylbutan-1-amine (0.2 mL). The mixture was heated at reflux for 24 h and upon cooling to room temperature was diluted with ether and washed with brine (3×30 mL). The solution was dried (Na2SO4) and concentrated and the residue chromatographed using ethyl acetate-hexane (40:60) as eluant. From the early fractions 97 mg of pure product was obtained.

1. temperatureThe mixture was heated
2. temperatureat reflux for 24 h
3. washwashed with brine (3×30 mL)
4. dry with materialThe solution was dried (Na2SO4)
5. concentrationconcentrated
6. customthe residue chromatographed

ORD-Eintrag

ord-453eba706ba8470a87c049c94fe88b57

Quelldatensatz

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07981900B2