Potassium Carbonate → HCID 46311864, Verbindung

Temperatur

78 °C

To a mixture of 3-fluorophenylboronic acid (1.6 g, 12 mmol), S—PHOS (0.304 g, 0.74 mmol), potassium carbonate (3.41 g, 25 mmol), 2-chloro-6-methylpyridin-3-amine 16 (1.3 g, 9.1 mmol), and Pd(OAc)2 (0.085 g, 0.38 mmol) was added acetonitrile (14 mL) and water (9 mL). The reaction mixture was degassed by bubbling nitrogen through the solution for 10 min and the reaction mixture was heated to 78° C. After 4 h, the reaction mixture was diluted with EtOAc, washed with brine (1×), dried over MgSO4, filtered, and concentrated. Purification by flash column chromatography on silica gel (10% to 50% EtOAc in hexanes) gave 2-(3-fluorophenyl)-6-methylpyridin-3-amine.

1. customThe reaction mixture was degassed
2. customby bubbling nitrogen through the solution for 10 min
3. additionthe reaction mixture was diluted with EtOAc
4. washwashed with brine (1×)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by flash column chromatography on silica gel (10% to 50% EtOAc in hexanes)

ORD-Eintrag

ord-bf74b374d36e48aba7bccd73ffa7a023

Quelldatensatz

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08791147B2