反应详情

温度

65 °C

To a solution of 0.700 g (1.56 mmol) N-[6-chloro-4-(2-chloro-phenyl)-pyridin-3-yl]-2-(3-chloro-5-hydroxy-phenyl)-N-methyl-isobutyramide in 10 ml N,N-Dimethylformamide 0.215 g (1.56 mmol) K2CO3 and 0.2 ml (1.56 mmol) ethyl chlordifluoroacetate was added and the resulting suspension heated at 65° C. for 15 h. After cooling to ambient temperature, the reaction mixture was poured into 75 ml water and extracted three times with 80 ml CH2Cl2. The combined organic solvents were dried (Na2SO4), filtered and evaporated. The residue was purified by flash-chromatography (SiO2, CH2Cl2/ethyl acetate 4:1) to give 0.38 g (49%) of the title compound as a white solid.

1. temperatureAfter cooling to ambient temperature
2. extractionextracted three times with 80 ml CH2Cl2
3. dry with materialThe combined organic solvents were dried (Na2SO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by flash-chromatography (SiO2, CH2Cl2/ethyl acetate 4:1)