1. A method for manufacturing a solid electrolyte with high ion-conductivity comprising a hybrid compound which contains at least polyvinyl alcohol and a zirconic acid compound as constituents, comprising the steps of hydrolyzing a zirconium salt or an oxyzirconium salt in a solution comprising a solvent including water, polyvinyl alcohol, and the zirconium salt or the oxyzirconium salt, removing the solvent, and contacting with alkali.
2. A method for manufacturing a solid electrolyte with high ion-conductivity comprising a hybrid compound which contains at least polyvinyl alcohol and a zirconic acid compound as constituents, comprising the steps of hydrolyzing a zirconium salt or an oxyzirconium salt by heating a solution comprising a solvent including water, polyvinyl alcohol, and the zirconium salt or the oxyzirconium salt to 50\xb0 C. or higher, removing the solvent; and contacting with alkali.
3. A method for manufacturing a high ion-conducting solid electrolyte with high ion-conductivity comprising a hybrid compound which contains at least polyvinyl alcohol and a zirconic acid compound as constituents, comprising the steps of hydrolyzing a zirconium salt or an oxyzirconium salt by heating a solution comprising a solvent including water, polyvinyl alcohol, and the zirconium salt or the oxyzirconium salt to 50\xb0 C. or higher at a pH of 7 or less, removing the solvent, and contacting with an alkali.
The claims below are in addition to those above.
All refrences to claim(s) which appear below refer to the numbering after this setence.
1. A crystalline polymorph of Levalbuterol hydrochloride, Form B, characterized by
X-ray diffraction peaks at 8.7, 14.5, 19.0, and 19.6 degree two-theta, \xb10.2 degree two-theta.
2. The crystalline polymorph of levalbuterol hydrochloride Form B according to claim 1 further characterized by x-ray diffraction peaks at 20.6, 22.6, 30.9, and 35.0 degree two-theta, \xb10.2 degree two-theta.
3. The crystalline polymorph of levalbuterol hydrochloride Form B according to claim 1 further characterized by IR peaks at 2970, 2802, 1615, 1599, 1560, 1546, 1507, 1482, 1444, 1364, 1313, 1199, 1151, 1111, 1094, 1034, 992, 829, 697, 653, 597, 537, and 454 cm\u22121.
4. A process for preparing levalbuterol hydrochloride Polymorph B characterized by X-ray diffraction peaks at 8.7, 14.5, 19.0, and 19.6 degree two-theta, \xb10.2 degree two-theta, said process comprising:
suspending or forming a slurry of the R enantiomer of albuterol dibenzoyl tartrate complex in at least one solvent;
adding hydrogen chloride in a C1-C4 alcohol to the suspension or slurry until levalbuterol hydrochloride Polymorph B is obtained; and
isolating the levalbuterol hydrochloride Polymorph B;
wherein the at least one solvent includes at least one linear or branched C3-C10 ester, linear or branched C3-C10 ketone, linear or branched C3-C10 ether, C6-C10 aromatic hydrocarbon, linear or branched C1-C4 alcohol, dimethylsulfoxide, dimethylformamide, acetonitrile or dichloromethane.
5. The process according to claim 4 further comprising adding water to the organic solvent.
6. The process according to claim 4, wherein the solvent includes at least one of ethyl acetate, acetone, tetrahydrofuran, dimethylcarbonate, acetomtrile, toluene, xylene, methanol, ethanol, isopropanol, dimethylsulfoxide, or dimethylformamide.
7. The process according to claim 4, wherein the ratio of the organic solvent to the C1-C4 alcohol, which is added with the HCl, is about 90% to about 10% by volume.
8. The process according to claim 7, wherein the ratio of the organic solvent to the C1-C4 alcohol, which is added with the hydrogen chloride, is about 95% to about 5% by volume.
9. The process according to claim 7 or 8, wherein the organic solvent is ethyl acetate and the C1-C4 alcohol is methanol in a ratio of about 95% to about 5% by volume.
10. The process according to claim 4, wherein the reaction is carried out at temperature of about \u221210\xb0 C. to about 40\xb0 C.
11. The process according to claim 4, wherein the reaction is carried out at room temperature.
12. The process according to claim 4, wherein the hydrogen chloride is added as a solution or a gas in a C1-C4 alcohol.
13. The process according to claim 4, wherein the hydrogen chloride is added in an amount of about 1.2 equivalents of hydrogen chloride per equivalent of the R enantiomer of albuterol dibenzoyl tartrate complex.
14. The crystalline polymorph of levalbuterol hydrochloride Form B according to claim 1 further characterized by differential scanning calorimetry curves of small endothermic event in the temperature range of 144\xb0 C. to 169\xb0 C. and decomposition during melting in the temperature range of 181\xb0 C. to 188\xb0 C.
15. The crystalline polymorph of levalbuterol hydrochloride Form B according to claim 3 further characterized by infrared peaks at 3137, 2865, 2437, 2364, 1268, and 1071 cm\u22121.