反应详情

温度

85 °C

A mixture of 1-(4-(difluoromethoxy)phenyl)-2-(3-hydroxyphenyl)ethane-1,2-dione (2.75 g), N-methylguanidine hydrochloride (1.237 g) and sodium carbonate (2.20 g) in ethanol was heated at 85° C. for 8 h, cooled to room temperature and evaporated in vacuo. The resultant residue was partitioned between water and chloroform. The organic phase was separated, dried over Na2SO4 and evaporated to a light brown oil. The oil was purified by flash chromatography (silica gel) using step gradient elution (100% chloroform to 15% methanol/chloroform) to afford the title compound as a white foamy glass, 2.20 g; 1H NMR (DMSO-d6): δ 9.24 (bs, 1H), 7.42 (d, J=8.8 Hz, 2H), 7.12 (t, J=74.3 Hz, 1H), 7.06 (d, J=8.8 Hz, 2H), 7.02 (m, 1H), 6.80 (m, 2H), 6.57 (bs, 2H), and 6.56 (m, 1H); MS (APPI) m/z 348.

1. temperaturecooled to room temperature
2. customevaporated in vacuo
3. customThe resultant residue was partitioned between water and chloroform
4. customThe organic phase was separated
5. dry with materialdried over Na2SO4
6. customevaporated to a light brown oil
7. customThe oil was purified by flash chromatography (silica gel)
8. washstep gradient elution (100% chloroform to 15% methanol/chloroform)