تفاعل #501399

معادلة التفاعل

8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

3-(2-fluoroethylaminomethyl)pyrrolidine

1,8-diazabicyclo[5,4,0]-7-undecene

→

title compound

المردود 14.1%

8-Chloro-1-cyclopropyl-6-fluoro-7-[3-(2-fluoroethyl)aminomethyl-1-pyrrolidinyl]-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

المردود 14.1%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed for an hour
2. 2
   درجة الحرارةAfter cooling
3. 3
   تركيزthe reaction mixture was concentrated and to the residue
4. 4
   workup.ADDITIONwas added acetonitrile-ether (1:1, 5 ml)
5. 5
   ترشيحthe resulting precipitate was collected by filtration
6. 6
   أخرىrecrystallized from chloroform-methanol-ether

الإجراء التجريبي

A suspension of 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (200 mg), 3-(2-fluoroethylaminomethyl)pyrrolidine (165 mg) and 1,8-diazabicyclo[5,4,0]-7-undecene (DBU, 100 mg) in absolute acetonitrile (2 ml) was refluxed for an hour. After cooling, the reaction mixture was concentrated and to the residue was added acetonitrile-ether (1:1, 5 ml). The solution was allowed to stand overnight at 5° C., then the resulting precipitate was collected by filtration and recrystallized from chloroform-methanol-ether to give the title compound (40 mg), mp 138°-142° C.

المصدر