反应详情

温度

150 °C

Into 180 mL of DMSO, 10.5 g (44.6 mmol) of Compound E and 19.2 g (223 mmol) of piperazine were dissolved, followed by stirring at 150° C. for about 2 hours. After completion of the reaction, the solvent was evaporated under reduced pressure, water was added to the residue, and the mixture was extracted with chloroform. The organic layer was washed with water and brine, and then dried over anhydrous magnesium sulfate. After evaporation of the solvent, the resulting residue was purified by silica gel column chromatography (23% aqueous ammonia/methanol/chloroform=1/10/90) and then recrystallized from ethyl acetate to obtain 9.91 g of Compound F as a white solid (yield: 78%).

1. customAfter completion of the reaction
2. customthe solvent was evaporated under reduced pressure, water
3. additionwas added to the residue
4. extractionthe mixture was extracted with chloroform
5. washThe organic layer was washed with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customAfter evaporation of the solvent
8. customthe resulting residue was purified by silica gel column chromatography (23% aqueous ammonia/methanol/chloroform=1/10/90)
9. customrecrystallized from ethyl acetate