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In ethanol; for 24 - 72h;Product distribution / selectivity;
Example 1; Ciprofloxacin hydrochloride monohydrate (50.2 g, 130 mmol) was suspended in absolute ethanol (350 mL) and vigorously stirred for 24 hours. The solids were collected by filtration and dried under vacuum at 60 C. to give anhydrous ciprofloxacin hydrochloride as a white solid (41.9 g, 114 mmol, 88% yield), giving the IR spectrum shown in FIG. 1 and the powder X-ray diffraction pattern of FIG. 3, bottom trace, peaks as listed on FIG. 4. The absence of any peaks attributable to hydration or solvent residue is to be noted.; Example 3; Ciprofloxacin hydrochloride monohydrate was placed in an open vial, which in turn was placed inside a closed jar containing absolute ethanol. After 3 days, analysis of the solid by powder X-ray diffraction showed complete conversion into anhydrous ciprofloxacin hydrochloride, 100% yield. The product gave the same IR and X-ray spectra as that of Example 1.
88%
In iso-butanol; for 2h;Product distribution / selectivity;
Example 2 Ciprofloxacin hydrochloride monohydrate (50.3 g, 130 mmol) was suspended in 2-butanol 350 mL and vigorously stirred for 2 hours. The suspension was then heated to reflux and 170 mL of liquid were distilled off. After cooling to room temperature, the solids were collected by filtration and dried under vacuum at 60 C. to give anhydrous ciprofloxacin hydrochloride as a white solid (42.3 g, 115 mmol, 88% yield). The product gave the same IR and X-ray spectra as that of Example 1.
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