反应详情

温度

50 °C

350 mg of ethyl 8-chloro-1-cyclopropyl-9-methyl-4-oxo-4H-quinolizine-3-carboxylate was dissolved in 3.5 ml of toluene. 1.8 ml of ethanol, 1.8 ml of 2 M aqueous sodium carbonate solution, 235 mg of 4-aminomethylphenylboronic acid hydrochloride and 40 mg of bis(triphenylphosphine)palladium (II) chloride were added to the obtained solution, and they were heated under reflux in argon atmosphere for 6 hours. The reaction mixture was acidified with 1 N hydrochloric acid. After washing the aqueous layer with ethyl acetate, it was taken and then concentrated under reduced pressure. 2 ml of methanol and 1 ml of 1 N sodium hydroxide were added to the obtained residue, and they were stirred at 50° C. for 1 hour. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in 10 ml of water and then neutralized with 1 N hydrochloric acid. The crystals thus formed were taken by the filtration to obtain 241 mg of 8-(4-aminomethylphenyl)-1-cyclopropyl-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid.

1. temperaturewere heated
2. temperatureunder reflux in argon atmosphere for 6 hours
3. washAfter washing the aqueous layer with ethyl acetate, it
4. concentrationconcentrated under reduced pressure
5. addition2 ml of methanol and 1 ml of 1 N sodium hydroxide were added to the obtained residue, and they
6. concentrationThe reaction mixture was concentrated under reduced pressure
7. dissolutionthe residue was dissolved in 10 ml of water
8. customThe crystals thus formed
9. filtrationwere taken by the filtration