Реакция #168641

Уравнение реакции

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

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

1-hydroxybenzotriazole

Diisopropylethylamine

methylhydroxyamine hydrochloride

→

title compound

Выход 77.6%

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

Выход 77.6%

Растворители

THF

Условия реакции

Обработка

1. 1
   ЭкстракцияThe resulting solution was extracted with ethylacetate
2. 2
   Промывкаwashed with salt solution
3. 3
   ДругоеThe resulting residue was recrystallized with diethylether

Методика

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%).

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