تفاعل #53453

معادلة التفاعل

isopropyl ether

3-Ethylaminoazetidine

1-(6-amino-3,5-difluoropyridin-2-yl)-8-bromo-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

N-methyl-pyrrolidine

→

title compound

المردود 77.6%

1-(6-amino-3,5-difluoropyridin-2-yl)-8-bromo-7-(3-ethylaminoazetidin-1-yl)-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

المردود 77.6%

المذيبات

dimethylsulfoxide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةto cool down
3. 3
   workup.STIRRINGthe mixture was stirred
4. 4
   أخرىa clear layer at the top of the mixture was removed
5. 5
   تركيزthe residue was concentrated under reduced pressure
6. 6
   workup.ADDITIONEthanol (5 mL) was added
7. 7
   درجة الحرارةthe mixture was heated
8. 8
   workup.STIRRINGunder stirring at 70° C. for 30 minutes
9. 9
   ترشيحThe precipitated solid was collected by filtration

الإجراء التجريبي

3-Ethylaminoazetidine (700 mg), 1-(6-amino-3,5-difluoropyridin-2-yl)-8-bromo-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (1.5 g), N-methyl-pyrrolidine (2.0 g)and dimethylsulfoxide (4.5 g) were combined, and the mixture was heated under stirring at 40° C. for 24 hours. After the mixture was allowed to cool down, isopropyl ether (10 mL) was added, the mixture was stirred, and a clear layer at the top of the mixture was removed. The same procedure was repeated once more, and the residue was concentrated under reduced pressure. Ethanol (5 mL) was added, and the mixture was heated under stirring at 70° C. for 30 minutes. The precipitated solid was collected by filtration. The title compound (1.38 g) was obtained.

المصدر