Crystals of laquinimod sodium and improved process for the manufacture thereof
a technology of laquinimod sodium and crystals, which is applied in the field of crystals of laquinimod sodium and improved process for the manufacture of thereof, can solve the problems of reducing the quality of crystalline characteristics and specifically tapped density
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Example 1
[0596]The pilot scale process of recrystallization of laquinimod sodium was based on Example 15 of U.S. Pat. No. 7,884,208. The starting material was crude laquinimod sodium having low particle size (d(0.1)=1-2μ, d(0.5)=6-11μ; d(0.9)=20-35μ) and appears as aggregated solid. Example 15 of U.S. Pat. No. 7,884,208 involves 25.0 g of laquinimod sodium (laboratory scale) prepared according to the method disclosed in U.S. Pat. No. 6,875,869. In Example 15, the 25.0 g of laquinimod sodium is dissolved in an aqueous solution of laquinimod sodium and then evaporated under vacuum at stirring to a concentrated solution having a volume ratio of 2.14 v / w, the resulting residue is seeded to induce crystallization then treated with an anti-solvent (acetone).
[0597]The modified pilot scale process was performed with 2.5 kg of laquinimod sodium which is a 100-fold scale up from Example 15. In addition, the modified pilot scale process had significant differences from t...
example 2
Recrystallization of Laquinimod Sodium—Laboratory Scale (Laboratory Scale Batch A)
[0602]Recrystallization of laquinimod sodium was performed on laboratory scale (Batch A) as follows.
[0603]All operations of Laquinimod Na re-crystallization step including evaporation were performed on laboratory scale in transparent agitated glass reactors equipped with stirrer, thermometers and circulating bath for heating and cooling.
[0604]25 g crude Na Laquinimod and 275 ml deionized water introduced into 250 ml stirred jacketed glass reactor. The mixture is stirred and heated to 70° C., after complete dissolution of the solid the solution is filtered through paper filter. Resulting clear filtrate introduced to 250 ml jacketed glass reactor equipped with circulating bath, stirrer, thermometer and vacuum distillation system.
[0605]Vacuum is applied and water is distilled at stirring, pressure during the evaporation is 38-40 mbar and jacket temperature is 55° C.
[0606]After distillation of ca. ⅔ volume...
example 3
Recrystallization of Laquinimod Sodium—Laboratory Scale (Laboratory Scale Batch B)
[0615]Recrystallization of laquinimod sodium was performed on laboratory scale (Batch B) as follows.
[0616]All operations of Laquinimod Na re-crystallization step including evaporation were performed on laboratory scale in transparent agitated glass reactors equipped with stirrer, thermometers and circulating bath for heating and cooling.
[0617]25 g Na Laquinimod crude and 275 ml deionized water introduced into 250 ml stirred jacketed glass reactor. The mixture is stirred and heated to 70° C., after complete dissolution of the solid the solution is filtered through paper filter. Resulting clear filtrate introduced to 250 ml jacketed glass reactor equipped with circulating bath, stirrer, thermometer and vacuum distillation system. Vacuum is applied and water is distilled at stirring, pressure during the evaporation is 38-40 mbar and jacket temperature is 55° C. During the distillation spontaneous crystall...
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