反应详情

温度

80 °C

A mixture of 3-amino-2-(2-chloro-5-methoxyphenyl)-7-hydroxy-2,5-dihydro-4H-pyrazolo[4,3-c]quinolin-4-one (75 mg), 1-(3-chloropropyl)-4-methylpiperazine dihydrochloride (70 mg), potassium carbonate (112 mg), potassium iodide (5 mg) and N,N-dimethylformamide (3 ml) was stirred at 80° C. for 4 hours. To the reaction mixture was added water, extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. To the concentrated residue (53 mg) was added DL-methilonine (265 mg) and methanesulfonic acid (3 ml), and the mixture was stirred at 90° C. for one night. The reaction mixture was cooled and then pH of the reaction mixture was adjusted to about 9 by adding an aqueous 20% sodium hydroxide and 5% sodium hydrogen carbonate, and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue was purified with propylaminated silica gel column chromatography to obtain the target compound (13 mg).

1. extractionextracted with ethyl acetate
2. washThe extract was washed with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. additionTo the concentrated residue (53 mg) was added DL-methilonine (265 mg) and methanesulfonic acid (3 ml)
6. stirringthe mixture was stirred at 90° C. for one night
7. temperatureThe reaction mixture was cooled
8. additionby adding an aqueous 20% sodium hydroxide and 5% sodium hydrogen carbonate
9. extractionextracted with ethyl acetate
10. washThe extract was washed with brine
11. dry with materialdried over anhydrous sodium sulfate
12. distillationthe solvent was distilled off under reduced pressure
13. customThe residue was purified with propylaminated silica gel column chromatography