反应详情

温度

90 °C

A mixture of 5-acetyl-2-acetylamino-4-trifluoromethyl-benzoic acid methyl ester (2.46 g, 8.1 mmol) and N,N dimethyl formamide dimethyl acetal (1.1 mL, 8.1 mmol) was stirred at 90° C. for 4 h. The mixture was diluted with AcOEt. The organic phase was washed with water, dried (Na2SO4) and concentrated in vacuo to afford a yellow paste. The crude product was purified by flash chromatography (silica gel, EtOAc/hexanes (50:50 to 100:0)) to provide the title compound as a beige paste (1.12 g, 39%). ES-MS: m/z 359.3 [M+H]+, rt 4.77 min.

1. washThe organic phase was washed with water
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated in vacuo
4. customto afford a yellow paste
5. customThe crude product was purified by flash chromatography (silica gel, EtOAc/hexanes (50:50 to 100:0))