Multistage process for preparation of highly pure deferoxamine mesylate salt
A technology of mesylate and deferoxamine, applied in the field of preparation of high-purity deferoxamine B mesylate, can solve problems such as overestimation of deferoxamine
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Embodiment 1
[0049] Crude deferoxamine B hydrochloride (7.88 kg) containing 5.30 kg of deferoxamine B was dissolved in water (362 L). Then at 14Lh -1 At a flow rate, pass the aqueous solution through an equal volume of Diaion packed in a 10-liter column SP 207 adsorption resin (Mitsubishi Chemical Corp.). The eluate contained 5.04 kg deferoxamine. Then, stir with 5gL -1 The amount of ammonium chloride was added to the eluent until the ammonium chloride was completely dissolved. The solution was then loaded into the Amberlite-containing XAD 1180 adsorption resin (132 L) (Rohm & Haas) was applied to a column and the bed was eluted with brine. The column was first eluted with 10% acetonitrile-water, then in 14Lh -1 Elute with 20% acetonitrile-water at a constant flow rate. Collect eluate fractions. The main fraction yielded a solution of deferoxamine hydrochloride containing 4.53 kg of deferoxamine B. The main fraction was then treated with activated carbon (45 g) and H + Form D...
Embodiment 2
[0053] Crude deferoxamine B hydrochloride (707 g) containing 587 g of deferoxamine B was dissolved in water (10 L). Then at 0.35Lh -1 At a flow rate, pass the aqueous solution through the Column with SP 207 Adsorbent Resin (1L). The eluate from the column was found to contain 562 grams of deferoxamine B. The eluent is then loaded onto the Amberlite packed in a column A bed of XAD 1180 adsorbent resin (7.2 L). First use 5.6L with a concentration of 10gL -1 Ammonium chloride aqueous solution in 0.7Lh -1 The bed was eluted at flow rate and then with a 1:4 methanol-water mixture. A single fraction of deferoxamine B (432 g) was collected. Fractions were decolorized by stirring with charcoal (40 g) and filtered. Evaporate the eluate after decolorization so that the concentration of deferoxamine B is 60gL -1 .
[0054] An equal amount of acetonitrile was then added. Concentrated aqueous ammonia was then added until the pH of the solution reached 9.8. 4 times the amoun...
Embodiment 3
[0056] Crude deferoxamine B hydrochloride (760 g) containing 530 g of deferoxamine B was dissolved in 1:1 acetonitrile-water (14 L) at 40°C. The resulting solution was then filtered and the pH was adjusted to 9.9 by the addition of concentrated aqueous ammonia. Acetonitrile (49 L) was added to precipitate deferoxamine B free base. The resulting suspension was cooled to 17°C and maintained at reduced temperature for 4 hours. The precipitate was isolated by filtration, washed with acetonitrile, and dried under reduced pressure to give deferoxamine B free base (403 g). The base was then suspended in water (20 L) and hydrochloric acid was added slowly until the base dissolved and the pH of the resulting solution reached 5.0-5.5.
[0057] Load the solution onto the Amberlite packed in a column XAD 1180 was adsorbed onto the bed of resin (7.2 L) and eluted with 25% acetonitrile-water. A single fraction of deferoxamine B (320 g) was obtained. The eluate containing deferoxamine...
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