Reacción #168641

Ecuación de reacción

5-amino-2,4-difluoro-benzoic acid

1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride

1-hydroxybenzotriazole

Diisopropylethylamine

methylhydroxyamine hydrochloride

→

title compound

Rendimiento 77.6%

5-amino-2,4-difluoro-N-methyl-benzamide

Rendimiento 77.6%

Disolventes

THF

Condiciones de reacción

Tratamiento posterior

1. 1
   ExtracciónThe resulting solution was extracted with ethylacetate
2. 2
   Lavadowashed with salt solution
3. 3
   OtroThe resulting residue was recrystallized with diethylether

Procedimiento

5-amino-2,4-difluoro-benzoic acid (6 g, 34.6 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (13.3 g, 69.3 mmol) and 1-hydroxybenzotriazole (9.3 g, 69.3 mmol) was stirred in THF (100 ml). Diisopropylethylamine (7.2 ml, 41.5 mmol) and methylhydroxyamine hydrochloride (4.3 g, 51.9 mmol) were added thereto, and the solution was stirred for 5 hours. The resulting solution was extracted with ethylacetate and washed with salt solution. The resulting residue was recrystallized with diethylether to obtain the title compound 5 g (yield: 71%).

Fuente