反应详情

温度

85 °C

Ethyl 8-chloro-1-ethyl-6,7,8,9-tetrafluoro-4H-quinolizin-4-one-3-carboxylate (317 mg, 1.0 mmol), from Step 4, is dissolved in 5 mL of dry pyridine under a nitrogen atmosphere. To the resultant solution is added 2 mL (2.0 mmol) of N-methylpiperazine and the stirred reaction mixture is heated at 85° C. for 2.5 hours. The reaction mixture is allowed to cool to ambient temperature and then concentrated in vacuo in order to remove all of the pyridine. The residue is dissolved in 50 mL of methylene chloride and the methylene chloride solution is washed with 50 mL of 5% aqueous sodium bicarbonate solution. The aqueous layer is extracted with 3 X 50 mL of methylene chloride and the combined methylene chloride solutions are dried over anhydrous sodium sulfate, filtered and concentrated and dried in vacuo to afford the title compound.

1. customthe stirred reaction mixture
2. temperatureto cool to ambient temperature
3. concentrationconcentrated in vacuo in order
4. customto remove all of the pyridine
5. dissolutionThe residue is dissolved in 50 mL of methylene chloride
6. washthe methylene chloride solution is washed with 50 mL of 5% aqueous sodium bicarbonate solution
7. extractionThe aqueous layer is extracted with 3 X 50 mL of methylene chloride
8. dry with materialthe combined methylene chloride solutions are dried over anhydrous sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated
11. customdried in vacuo