Reaktion #2504045

Reaktionsgleichung

Carbonyldiimidazole

2-(2,4-difluoroanilino)-4,5-difluorobenzoic acid

O-Benzylhydroxylamine hydrochloride

triethylamine

→

title compound

Ausbeute 91.2%

N-Benzyloxy-2-(2,4-difluoroanilino)-4,5-difluoro-benzamide

Ausbeute 91.2%

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturto reflux for 4 hours
3. 3
   EinengenThe reaction mixture was concentrated
4. 4
   Waschenwashed with 1N HCl, saturated NaHCO3, brine
5. 5
   Trocknendried over magnesium sulfate
6. 6
   EinengenThe solution was concentrated

Vorschrift

Carbonyldiimidazole (3.1 g, 19.1 mmol) was added to a suspension of 2-(2,4-difluoroanilino)-4,5-difluorobenzoic acid (Example H-4, 4.54 g, 15.9 mmol) in 120 mL of THF, and the mixture was stirred for 24 hours at 25° C. O-Benzylhydroxylamine hydrochloride (2.54 g, 15.9 mmol) and triethylamine (2.66 mL, 19.1 mmol) were added, and the mixture was heated to reflux for 4 hours. The reaction mixture was concentrated and washed with 1N HCl, saturated NaHCO3, brine, and dried over magnesium sulfate. The solution was concentrated to give 5.66 g of the title compound as an oil.

Quelle