反应详情

To a solution of the compound obtained in Step 2 (1.20 g, 4.34 mmol), 9-ethyl-9H-carbazol-3-amine (0.913 g, 4.34 mmol) and DIEA (1.896 mL, 10.86 mmol) in DMF (15 mL) was added HATU (1.982 g, 5.21 mmol), and the mixture was stirred at room temperature for 4 hr. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (solvent gradient; 10 to 85% ethyl acetate/hexane), and purified by NH-silica gel column chromatography (solvent gradient; 10 to 100% ethyl acetate/hexane) to give the title compound (0.788 g, 1.681 mmol, 38.7%) as a colorless powder.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with water and saturated brine
3. customdried
4. customthe solvent was evaporated under reduced pressure
5. customThe obtained residue was purified by silica gel column chromatography (solvent gradient; 10 to 85% ethyl acetate/hexane)
6. custompurified by NH-silica gel column chromatography (solvent gradient; 10 to 100% ethyl acetate/hexane)