2-Morpholinoethanol → HCID 9829665, compound

Participants

Reaction Steps

In 3 l of methylene chloride were added 58.94 g (0.127 mole) of 1-ethyl-6-fluoro-8-difluoromethoxy-7-[4-(2-pyrimidinyl)piperazin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 25.05 g (0.191 mole) of 4-(2-hydroxyethyl)morpholine, 23.3 g (0.191 mole) of 4-dimethylaminopyridine and 48.8 g (0.254 mole) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride, and the mixture was stirred at room temperature for 4 days. Then, the solvent was removed under reduced pressure. The residue was dissolved in chloroform, washed with a 1N hydrochloric acid aqueous solution, washed with water and dried. The solvent was removed under reduced pressure, and the residue was applied to silica gel column chromatography (the eluent used was a mixture of chloroform: methanol: 28% aqueous ammonia=40:9:1) to obtain 50.25 g of the title compound as slightly yellowish white powder.

Provenance & Evidence