Reaktion #521869

Reaktionsgleichung

piperidine

8,9-dichloro-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid

piperidine

→

9-chloro-8-(1-piperidyl)-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid

Ausbeute 24.4%

Lösungsmittel

hexamethylphosphoric triamide

hexamethylphosphoric triamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe mixture was reacted at 160° C. on an oil bath for 5 hours
2. 2
   workup.DISTILLATIONwere distilled off under reduced pressure and to the residue
3. 3
   workup.ADDITIONwas added ethyl acetate
4. 4
   Sonstigecrystallized
5. 5
   SonstigeRecrystallization from dimethylformamide-water

Vorschrift

In a 200 ml autoclave were placed 4.6 g of 8,9-dichloro-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid, 5 g of piperidine and 50 ml of hexamethylphosphoric triamide and the mixture was reacted at 160° C. on an oil bath for 5 hours. After completion of reaction hexamethylphosphoric triamide and piperidine were distilled off under reduced pressure and to the residue was added ethyl acetate and crystallized. Recrystallization from dimethylformamide-water give 1.3 g of 9-chloro-8-(1-piperidyl)-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid. m.p. 246° to 248° C.

Quelle