Phosphorus oxychloride → 2177297-18-4

Reaktionsgleichung

[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([NH2:9])=[C:4]([F:10])[CH:3]=1.[CH:11]([NH:14][C:15](=O)[CH3:16])([CH3:13])[CH3:12].P(Cl)(Cl)(Cl)=O>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([NH:9][C:15](=[N:14][CH:11]([CH3:13])[CH3:12])[CH3:16])=[C:4]([F:10])[CH:3]=1

Komponenten

Versuchsvorschrift

Add TEA (10.05 mL) to a mixture of 4-bromo-2,6-difluoro-phenylamine (10.0 g), N-isopropyl acetamide (9.73 g), phosphoryl chloride (6.70 mL) in toluene (150 mL). Heat the mixture to reflux for 3 h. Cool the mixture and remove the solvent under vacuum. Dissolve the crude in DCM, wash with an aqueous saturated solution of sodium bicarbonate several times to remove all traces of acid. Dry over sodium sulfate and remove the solvent under vacuum to afford 14 g of the title compound. MS (ES+): m/z=292 (M+H)+.