N-异丙基氮杂环丁烷-3-胺二盐酸盐

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N-isopropylazetidin-3-ylamine dihydrochloride (374 mg), 1-(6-amino-3,5-difluoropyridin-2-yl)-8-bromo-6,7-difluoro-4-oxo-1,4-dihydroquinolin-3-carboxylic acid (518 mg), N-methylpyrrolidine (0.8 mL), lithium chloride (500 mg) and dimethyl sulfoxide (1.5 mL) were mixed, and the mixture was stirred at 50° C. for 4.5 hours. After the mixture had been left to cool, diethyl ether (10 mL) was added to the mixture and stirred, followed by removing the supernatant. The same procedure was repeated three times. Water (3 mL) was added to the residue, and the pH of the mixture was adjusted to 6 by use of aqueous citric acid solution. The formed solid was collected through filtration, washed three times with water (3 mL), then suspended in ethanol (10 mL), and stirred under heating. The formed solid was collected through filtration, and suspended in diisopropyl ether (10 mL), followed by stirring under heating. The heated suspension was filtrated to yield 410 mg of the title compound. After the mixture had been left to cool stirred by removing the supernatant Water (3 mL) was added to the residue The formed solid was collected through filtration washed three times with water (3 mL) stirred under heating The formed solid was collected through filtration by stirring under heating The heated suspension was filtrated

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N-isopropylazetidin-3-ylamine dihydrochloride (374 mg), 1-(6-amino-3,5-difluoropyridin-2-yl)-8-bromo-6,7-difluoro-4-oxo-1,4-dihydroquinolin-3-carboxylic acid (518 mg), N-methylpyrrolidine (0.8 mL), lithium chloride (500 mg) and dimethyl sulfoxide (1.5 mL) were mixed, and the mixture was stirred at 50° C. for 4.5 hours. After the mixture had been left to cool, diethyl ether (10 mL) was added to the mixture and stirred, followed by removing the supernatant. The same procedure was repeated three times. Water (3 mL) was added to the residue, and the pH of the mixture was adjusted to 6 by use of aqueous citric acid solution. The formed solid was collected through filtration, washed three times with water (3 mL), then suspended in ethanol (10 mL), and stirred under heating. The formed solid was collected through filtration, and suspended in diisopropyl ether (10 mL), followed by stirring under heating. The heated suspension was filtrated to yield 410 mg of the title compound. After the mixture had been left to cool stirred by removing the supernatant Water (3 mL) was added to the residue The formed solid was collected through filtration washed three times with water (3 mL) stirred under heating The formed solid was collected through filtration by stirring under heating The heated suspension was filtrated