反应详情

温度

-10 °C

The deferoxamine free base was suspended in a 14:3 mixture of ethanol and water (42.5 L). Dilute methanesulfonic acid was slowly added to the suspension until the free base dissolved and the solution attained a pH of between 3.7 and 5. Ethanol (200 L) was added to the solution to precipitate the mesylate salt and the resulting suspension was cooled to −10° C. and maintained at −10° C. for several hours. The resulting crystals were isolated by filtration, washed with ethanol (50 L) and dried under vacuum to yield 3.4 kg of deferoxamine mesylate. HPLC chromatography showed that the mesylate contained 1.84 weight % impurities. The moisture content as determined by Karl-Fischer Analysis was 0.2 mole %. USP/NF 24/19, pp. 2003-2004 (1999). Coloration was better than Y5 as measured according to the European Pharmacopeia criteria for grading coloration.

1. dissolutiondissolved
2. customto precipitate the mesylate salt
3. temperaturemaintained at −10° C. for several hours
4. customThe resulting crystals were isolated by filtration
5. washwashed with ethanol (50 L)
6. customdried under vacuum