Water → HCID 18549167, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of 1.5 g of ethyl 1-(2,4-difluorophenyl)-7,8,9-trifluoro-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylate and 1.8 g of 4-(4-fluorophenyl)piperazine in 20 cm3 of dimethyl sulphoxide was heated, with stirring, at a temperature around 100° C. for approximately 1 hour. After cooling to approximately 20° C., the reaction mixture was poured into 100 cm3 of water and extracted 3 times with 50 cm3 of trichloromethane. The combined organic extracts were washed 1 time with 50 cm3 of water, dried over magnesium sulphate and concentrated under reduced pressure (20 kPa) at a temperature around 40° C. 1.7 g of ethyl 7,9-difluoro-1-(2,4-difluorophenyl)-8-[4-(4-fluorophenyl)piperazin-1-yl]-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylate were obtained in the form of a yellow solid melting at about 298-299° C., which solid was used without additional purification in the subsequent stages.

Provenance & Evidence