反应详情

To a solution of (2E)-3-{1-[bis(4-fluorophenyl)methyl]-3-cyano-4,6-dimethyl-1H-pyrrolo[2,3-b]pyridin-2-yl}prop-2-enoic acid (250 mg, 0.570 mmol) in THF (2.5 ml) were added DMF (0.025 ml) and oxalylchloride (0.060 ml, 0.680 mmol), the mixture was stirred at room temperature for 1 hour and the solvent was distilled off under reduced pressure. The residue was added under ice-cooling to a solution of morpholine (0.0985 ml, 1.13 mmol), triethylamine (0.314 ml, 2.26 mmol) and THF (2.5 ml), and the mixture was stirred under ice-cooling for 2 hours and at room temperature for 12 hours. The reaction solution was poured into water and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent distilled off under reduced pressure. The residue was recrystallized from hexane and ethyl acetate to give the objective product as a solid material.

1. distillationthe solvent was distilled off under reduced pressure
2. additionThe residue was added under ice-
3. stirringthe mixture was stirred under ice-
4. temperaturecooling for 2 hours and at room temperature for 12 hours
5. extractionextracted with ethyl acetate
6. washThe extract was washed with water
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationthe solvent distilled off under reduced pressure
9. customThe residue was recrystallized from hexane and ethyl acetate