Hydrochloric Acid → HCID 69997281, compound

Participants

Reaction Steps

16ar) A suspension of 0.33 g of 1-cyclohexyl-7-[5-(2,4-diamino-pyrimidin-5-ylmethyl)-2,3-dimethoxy-phenylethynyl]-6,8-difluoro-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid hydrochloride (Example 16aq)) in 5 ml of methanol is treated with 2 ml of 28% aqueous sodium hydroxide solution and held at reflux for 5 hrs. The beige suspension is cooled to room temperature and acidified with 25% aqueous hydrochloric acid. The precipitated substance is filtered off under suction, washed with 10 ml of water, 10 ml of ethanol and 10 ml of ether and dried. 0.264 g (78%) of 1-cyclohexyl-7-[5-(2,4-diamino-pyrimidin-5-ylmethyl)-2,3- dimethoxy-phenylethynyl]-6-fluoro-8-methoxy-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid hydrochloride is obtained as a beige solid. Yield: 78%. M.p.>205° (dec.). Mass spectrum (FAB): peaks inter alia at 602 (M++H, 100%), 588 (10%), 520 (7%).

Provenance & Evidence