反应详情

温度

140 °C

Into 7 mL of DMSO, 500 mg (2.12 mmol) of Compound E was dissolved, and then 0.95 mL (6.36 mmol) of DBU and 1.50 g (9.50 mmol) of 1-(2-hydroxy-2-methylpropyl)piperazine were added thereto, followed by stirring at 140° C. for about 2 hours. After completion of the reaction, the reaction mixture was extracted by adding chloroform and water, and 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 (3% methanol-chloroform) and then recrystallized from a mixed solvent of hexane-ethyl acetate to obtain 250 mg of Compound 1 as a white solid (yield: 33%).

1. customAfter completion of the reaction
2. extractionthe reaction mixture was extracted
3. additionby adding chloroform and water
4. washthe organic layer was washed with water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customAfter evaporation of the solvent
7. customthe resulting residue was purified by silica gel column chromatography (3% methanol-chloroform)
8. customrecrystallized from a mixed solvent of hexane-ethyl acetate