反应详情

温度

85 °C

A mixture of 4,4,4-Trifluoro-1-(4-fluoro-phenyl)-butane-1,3-dione (15 g, 64 mmol) and NBS (11.4 g, 64.1 mmol) was ground together at RT, which incited to give a homogeneous mixture and then solidified to give crude brominated product. Water was added to rinse the solid. The solid was taken up in ethanol (50 mL), and thiourea (4.9 g, 64 mmol) was added. The mixture was heated at 85° C. for 4 h, cooled to RT and partitioned between ethyl acetate and aq. K2CO3. The organic extract was dried over MgSO4, concentrated and chromatographed to give the title compound. m/z 291.0 (MH+).

1. customwas ground together at RT
2. customto give a homogeneous mixture
3. customto give crude brominated product
4. washto rinse the solid
5. temperaturecooled to RT
6. custompartitioned between ethyl acetate and aq. K2CO3
7. extractionThe organic extract
8. dry with materialwas dried over MgSO4
9. concentrationconcentrated
10. customchromatographed