反应详情

温度

140 °C

4-Chloro-2-methylquinoline (1.8 g, 10 mmol) and anhydrous piperazine (5.25 g, 60 mmol) were dissolved in ethyleneglycol monoethylether (15 ml) and stirred at 140° C. overnight. The mixture was concentrated under reduced pressure, toluene was added (2×100 ml) and the solvent removed under reduced pressure. To the residue was added 0.5 M NaOH (100 ml) and the mixture was extracted with a mixture of dichloromethane/diethylether/ethyl acetate (1:1:1, 3×100 ml). The combined organic phases were washed with brine, dried over sodium sulfate and the solvent was removed under reduced pressure. 2.78 g of an off-white solid (8.5 mmol, 85%) were obtained that were used directly in the next step.

1. concentrationThe mixture was concentrated under reduced pressure, toluene
2. additionwas added (2×100 ml)
3. customthe solvent removed under reduced pressure
4. additionTo the residue was added 0.5 M NaOH (100 ml)
5. extractionthe mixture was extracted with a mixture of dichloromethane/diethylether/ethyl acetate (1:1:1, 3×100 ml)
6. washThe combined organic phases were washed with brine
7. dry with materialdried over sodium sulfate
8. customthe solvent was removed under reduced pressure