تفاعل #168641

معادلة التفاعل

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

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

1-hydroxybenzotriazole

Diisopropylethylamine

methylhydroxyamine hydrochloride

→

title compound

المردود 77.6%

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

المردود 77.6%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   استخلاصThe resulting solution was extracted with ethylacetate
2. 2
   غسيلwashed with salt solution
3. 3
   أخرىThe resulting residue was recrystallized with diethylether

الإجراء التجريبي

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%).

المصدر