反应详情

温度

45 °C

Crude (2,3-difluoro-5-nitrophenyl)acetic acid (12, 1.00 g, 0.00461 mol) and a 40% solution of methylamine in water (3 eq., 1.20 ml, 0.0138 mol) are mixed in DMSO (5 ml) and stirred at 45° C. for 1 hour. 2N Hydrochloric acid (20 ml) is added in one portion and the mixture stirred at room temperature for 1 hour. The reaction mixture is extracted with ethyl acetate and the extract washed with saturated aqueous sodium bicarbonate and brine, dried (MgSO4) and evaporated. The residue is purified by flash column chromatography (50% ethyl acetate/hexane) to give the title compound as a solid. HPLC r.t. 4.4 min.

1. stirringthe mixture stirred at room temperature for 1 hour
2. extractionThe reaction mixture is extracted with ethyl acetate
3. washthe extract washed with saturated aqueous sodium bicarbonate and brine
4. dry with materialdried (MgSO4)
5. customevaporated
6. customThe residue is purified by flash column chromatography (50% ethyl acetate/hexane)