Dimethylformamide → 2,6-Dichloro-5-fluoronicotinamide

Temperatur

72 °C

To a suspension of 10 g of 2,6-dichloro-5-fluoronicotinic acid in 30 mL of toluene, 8.5 g of thionyl chloride and 0.10 mL of N,N-dimethylformamide were added, and the mixture was stirred at 72° C. for 1 hour 30 minutes. The reaction mixture was cooled to room temperature, and the solvent was distilled off under reduced pressure. The resultant residue was dropped to 30 mL of 25% ammonium water at −20° C. The temperature was increased to 5 C.°, and the mixture was stirred for 30 minutes. The solid was filtered off to obtain 9.9 g of 2,6-dichloro-5-fluoronicotinamide as a white solid.

1. additionwere added
2. temperatureThe reaction mixture was cooled to room temperature
3. distillationthe solvent was distilled off under reduced pressure
4. additionThe resultant residue was dropped to 30 mL of 25% ammonium water at −20° C
5. temperatureThe temperature was increased to 5 C.°
6. stirringthe mixture was stirred for 30 minutes
7. filtrationThe solid was filtered off

ORD-Eintrag

ord-9d88fa9534da41fba2bada2511e4ee59

Quelldatensatz

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08367831B2