반응 #168641

반응 방정식

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

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

1-hydroxybenzotriazole

Diisopropylethylamine

methylhydroxyamine hydrochloride

→

title compound

수율 77.6%

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

수율 77.6%

용매

THF

반응 조건

후처리

1. 1
   추출The resulting solution was extracted with ethylacetate
2. 2
   세척washed with salt solution
3. 3
   기타The resulting residue was recrystallized with diethylether

실험 절차

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%).

출처