Reaktion #1160940
ord-d60d70b378ba496e83784ec28ad6dcc9
Reaktionsgleichung
1-cyclopropyl-6-fluoro-7-bromo-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid
3-methylpiperazine
→
1-cyclopropyl-6-fluoro-7-(3-methyl-1-piperazinyl)-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid
Ausbeute 50.6%
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.DISTILLATIONAfter the solvent is distilled off under reduced pressure, ethanol
- 2workup.ADDITIONis added to the residue
- 3Sonstigethe crystals are separated by filtration
- 4Sonstigeare recrystallized from ethyl acetate-ethanol
Vorschrift
To a solution of 1-cyclopropyl-6-fluoro-7-bromo-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (0.58 g) in N-methyl-2-pyrrolidone (5 ml) is added 3-methylpiperazine (0.65 g), and the mixture is heated at 90° C. for 20 minutes. After the solvent is distilled off under reduced pressure, ethanol is added to the residue, and the crystals are separated by filtration and are recrystallized from ethyl acetate-ethanol to give 1-cyclopropyl-6-fluoro-7-(3-methyl-1-piperazinyl)-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (310 mg), as white powdery crystals, m.p. 206°-208° C.