反应详情

温度

130 °C

A mixture of cyclohexane-1,3-dione (2.00 g, 17.8 mmol), 4-amino-2-trifluormethylpyridine (2.89 g, 17.8 mmol) and glacial acetic acid (10 mL) is heated at 130° C. for 4 h. The mixture cooled at room temperature, diluted with ethyl acetate and extracted three times with water. The phases are separated, and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried over Na2SO4 and concentreated under reduced pressure. The residue is purified by flash chromatography on silica (gradient dichloromethane/is methanol 95:5). Yield: 940 mg; ESI mass spectrum [M+H]+=257; Retention time HPLC: 0.80 min (V011_S01).

1. temperatureThe mixture cooled at room temperature
2. extractionextracted three times with water
3. customThe phases are separated
4. extractionthe aqueous layer is extracted with ethyl acetate
5. dry with materialThe combined organic layers are dried over Na2SO4
6. customThe residue is purified by flash chromatography on silica (gradient dichloromethane/is methanol 95:5)
7. custom0.80 min (V011_S01)