反应详情

温度

85 °C

Ethyl 8-chloro-1-ethyl-4H-quinolizin-4-one-3-carboxylate (279 mg, 1.0 mmol), the product of Step 3 of Example 62, was dissolved in 5 mL of dry pyridine under a nitrogen atmosphere. To the resultant solution was added 2 mL (2.0 mmol) of N-methylpiperazine and the stirred reaction mixture was heated at 85° C. for 2.5 hours. The reaction mixture was allowed to cool to ambient temperature and then concentrated in vacuo in order to remove all of the pyridine. The residue was dissolved in 50 mL of methylene chloride and the methylene chloride solution was washed with 50 mL of 5% aqueous sodium bicarbonate solution. The aqueous layer was extracted with 3×50 mL of methylene chloride and the combined methylene chloride solutions were dried over anhydrous sodium sulfate, filtered and concentrated and dried in vacuo to afford 343 mg of the title compound, m.p. 94°-96° C.; MS DCI-NH3 : 344 (M+H)+.

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 was dissolved in 50 mL of methylene chloride
6. washthe methylene chloride solution was washed with 50 mL of 5% aqueous sodium bicarbonate solution
7. extractionThe aqueous layer was extracted with 3×50 mL of methylene chloride
8. dry with materialthe combined methylene chloride solutions were dried over anhydrous sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated
11. customdried in vacuo