تفاعل #460708

ord-28f97a0a52464ceab8e371799c8ee099

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةunder reflux for 5 hours
  3. 3
    تركيزThe reaction mixture was concentrated under reduced pressure
  4. 4
    workup.ADDITIONWater was added to the residue
  5. 5
    workup.ADDITIONtreated with activated charcoal
  6. 6
    أخرىThe crystals which precipitated
  7. 7
    ترشيحwere collected by filtration

الإجراء التجريبي

A mixture of 3.0 g of 5-benzylamino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 2.5 g of 2-methylpiperazine and 30 ml of pyridine was heated under reflux for 5 hours. The reaction mixture was concentrated under reduced pressure. Water was added to the residue, and the solution was acidified with acetic acid and treated with activated charcoal. It was then neutralized with aqueous ammonia. The crystals which precipitated were collected by filtration to give 2.9 g of 5-benzylamino-1-cyclopropyl-6-fluoro-7-(3-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid. m.p. 129°-130° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05164392uspto-grants-1992_11