反应详情

温度

50 °C

Crude (2,3-difluoro-5-nitrophenyl) acetic acid (2.00 g, 9.2 mmol) and n-propylamine (6 eq., 4.54 ml, 0.0553 mol) are mixed in DMSO (10 ml) and stirred at 50° C. for 2 hours. 2N Hydrochloric acid (40 ml) is added in one portion and the mixture stirred at room temperature for 2 hours. The resulting light yellow precipitate is filtered, washed with water and dried under vacuum. The residue is purified by flash column chromatography (20% Ethylacetate/hexane) to give the title compound as a yellow solid. HPLC r.t. 5.40 min; MS for C11H11FN2O3 m/z 239.1 (M+H)+.

1. stirringthe mixture stirred at room temperature for 2 hours
2. filtrationThe resulting light yellow precipitate is filtered
3. washwashed with water
4. customdried under vacuum
5. customThe residue is purified by flash column chromatography (20% Ethylacetate/hexane)