Dimethylformamide → HCID 22030088, Verbindung

Temperatur

0 °C

Heat a solution of 6′-chloro-3-trifluoromethyl-[2,3′]bipyridinyl-5′-ylamine (25 g, 0.091 mol), zinc cyanide (6.75 g, 0.058 mol), tris[dibenzylidineacetone]di-palladium (also referred to as “pd2(dba)3”; 2.63 g, 2.86 mmol), 1,1′-bis(diphenylphosphino)ferrocene (also referred to as “DPPF”; 3.16 g, 5.72 mmol) in DMF (250 mL) and water (2.5 mL), under a nitrogen atmosphere, at 120° C. for 1 hour. Add water (30 mL) and heat the solution at 120° C. for a further 4 hours to complete the hydrolysis. Cool the reaction to 0° C. and add a solution of saturated ammonium chloride (200 ml), water (200 mL) and concentrated ammonium hydroxide (50 mL). After stirring at 0° C. for 1 hour, filter the yellow precipitate, and wash with water (200 mL) and a 1:1 mixture of ether-hexane (200 mL). Dry the solid in air and then in a vacuum oven to give (23 g, 90%) of the title compound.

1. customthe hydrolysis
2. temperatureCool
3. customthe reaction to 0° C.
4. filtrationfilter the yellow precipitate
5. washwash with water (200 mL)
6. additiona 1:1 mixture of ether-hexane (200 mL)
7. customDry the solid in air

ORD-Eintrag

ord-b59ea10f78174340acb3669f5da7c0fb

Quelldatensatz

uspto-grants-2007_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07304059B2