Benzenamine, 3-(methylthio)- → HCID 11529322, Verbindung

To 2,6-dichloro-4-iodopyridine (1.3715 g, 5 mmol) dissolved in toluene (30 mL) were added 3-methylthioaniline (0.73 mL, 6 mmol), tris(dibenzylidene-acetone)dipalladium (90.6 mg, 0.1 mmol), 1,3-bis(diphenylphosphino)propane (80.0 mg, 0.2 mmol), and sodium-tert-butoxide (672.1 mg, 7 mmol). The resulting mixture was allowed to stir at reflux for 12-18 hours. The sample was diluted in dichloromethane and filtered through Celite™. The Celite™ was washed with dichloromethane and the filtrate was washed two times with water and one time with brine. The organic phase was dried over potassium carbonate and concentrated by rotary evaporation. The resulting sample (9) was dried for 12-18 hours under vacuum. The sample was used without purification.

1. temperatureat reflux for 12-18 hours
2. filtrationfiltered through Celite™
3. washThe Celite™ was washed with dichloromethane
4. washthe filtrate was washed two times with water and one time with brine
5. dry with materialThe organic phase was dried over potassium carbonate
6. concentrationconcentrated by rotary evaporation
7. dry with materialThe resulting sample (9) was dried for 12-18 hours under vacuum
8. customThe sample was used without purification

ORD-Eintrag

ord-49d992825ad2495da4b2436a5d76dd94

Quelldatensatz

uspto-grants-2009_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07622486B2