Hydrochloric Acid → 1-Cyclopropyl-7-[5-(2,4-diamino-pyrimidin-5ylmethyl)-2,3-dimethoxy-phenylethynyl]-6,8-difluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid hydrochloride

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Reaction Steps

0.51 g of ethyl 1-cyclopropyl-7-[5-(2,4-diamino-pyrimidin-5ylmethyl)-2,3-dimethoxy-phenylethynyl]-6,8-difluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylate (Example 12a)) is held at reflux in 7 ml of ethanol and 7 ml of a 2N aqueous sodium hydroxide solution for one hour. The reaction mixture is cooled to room temperature and acidified with 25% aqueous hydrochloric acid. The precipitated substance is filtered off under suction, washed with 20 ml of water, 20 ml of ethanol and 20 ml of ether and dried. 444 mg (86%) of 1-cyclopropyl-7-[5-(2,4-diamino-pyrimidin-5ylmethyl)-2,3-dimethoxy-phenylethynyl]-6,8-difluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid hydrochloride are obtained as a colourless solid. M.p.>230°. Mass spectrum (ISP): peaks: inter alia at 548.5 (M++H, 100%).

Provenance & Evidence