Reaktion #2358457

ord-2cee772da0e14e5f9d812df6f503c4a7

Reaktionsgleichung

Cl
hydrochloric acid
CCOC(=O)c1cn(C2CC2)c2cc(F)c(F)c(C)c2c1=O
ethyl 1-cyclopropyl-6,7-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylate
Cc1c(F)c(F)cc2c1c(=O)c(C(=O)O)cn2C1CC1
1-cyclopropyl-6,7-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid
Ausbeute 92.7%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturby refluxing for 2 hours
  2. 2
    TemperaturAfter cooling
  3. 3
    Sonstigethe crystals precipitated
  4. 4
    Filtrationwere collected by filtration
  5. 5
    Waschenwashed with water
  6. 6
    Waschenby washing with ethanol

Vorschrift

20 ml of 90% acetic acid and 5 ml of concentrated hydrochloric acid were added to 1.9 g of ethyl 1-cyclopropyl-6,7-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylate, followed by refluxing for 2 hours. After cooling, the crystals precipitated were collected by filtration and washed with water, followed by washing with ethanol and then with diethyl ether to give 1.6 g of 1-cyclopropyl-6,7-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06333431B1uspto-grants-2001_12