1. A crystalline form of fexofenadine free base characterized by a powder X-ray diffraction pattern with peaks at 11.9, 17.6, 18.2, 18.6, and 19.4\xb10.2 degrees two theta.
2. The crystalline fexofenadine free base of claim 1, further characterized by XRD peaks at 9.9, 13.7, 21.0, 21.8 and 22.7\xb10.2 degrees two theta.
3. The crystalline fexofenadine free base of claim 2, wherein the crystalline form has an X-ray powder diffraction diagram as substantially depicted in FIG. 1.
4. The crystalline form of fexofenadine free base of claim 1 having a DSC thermogram with endothermic peaks at about 102\xb0 C. and 142\xb0 C.
5. The crystalline form of fexofenadine free base of claim 1 having a TGA thermogram showing a weight loss of about 6-7% at a temperature range of about 25-120\xb0 C.
6. A process for preparing crystalline fexofenadine free base form of claim 1 comprising acidifying a basic aqueous solution of fexofenadine free base containing a mixture of water and an organic solvent to precipitate the crystalline form and recovering the crystalline form of fexofenadine free base.
7. The process of claim 6, wherein the organic solvent is a C1 to C4 alcohol.
8. The process of claim 7, wherein the alcohol is methanol.
9. The process of claim 6, wherein the acid is acetic acid.
10. A process for preparing fexofenadine HCl further comprising converting the fexofenadine free base of claim 6 to the HCl salt.
11. A process for preparing crystalline fexofenadine HCl salt comprising acidifying a basic aqueous solution of fexofenadine free base containing a mixture of water and an organic solvent to precipitate the crystalline form, and converting the crystal to the HCl salt.
12. A process for preparing crystalline fexofenadine free base of claim 1 comprising the steps of preparing a solution of fexofenadine keto acid in a water miscible organic solvent in the presence of a base and water; adding a reducing agent to the solution to reduce the keto-acid; acidifying reaction mixture obtained from the reduction to precipitate fexofenadine free base and recovering the crystalline form of fexofenadine free base.
13. The process of claim 12, wherein the water miscible organic solvent is selected from the group consisting of C1-C4 alcohols.
14. The process of claim 13, wherein the C1-C4 alcohol is methanol.
15. The process of claim 12, wherein the ratio of the water to the water miscible organic solvent is about 1:1 to about 1:6.
16. The process of claim 12, wherein the base is selected from the group consisting of: NaOH, KOH, NaOMe, NaOtBu and KOtBu.
17. The process of claim 16, wherein the base is NaOH.
18. The process of claim 12, wherein the reducing agent is selected from the group consisting of: sodium borohydride, potassium borohydride, lithium aluminium hydride (LiAlH4), and sodium cianoborohydride (NaBH3CN).
19. The process of claim 18, wherein the reducing agent is sodium borohydride.
20. The process of claim 12, wherein the reducing agent is added to the solution at a temperature of about 20\xb0 C. to about 35\xb0 C.
21. The process of claim 12, wherein the amount of the reducing agent is higher than about 1 equivalent.
22. The process of claim 21, wherein the amount of the reducing agent is about 1 to about 4 equivalents.
23. The process of claim 12, wherein the acid is selected from the group consisting of HCl, formic acid and acetic acid.
24. The process of claim 23, wherein the acid is acetic acid.
25. The process of claim 12, wherein acidifying is carried out to a pH of about 5 to about 9.
26. The process of claim 25, wherein acidifying is carried out to a pH of about 5 to about 6.5.
27. The process of claim 26, wherein acidifying is carried out to a pH of about 5.
28. The process of claim 12 further comprising adding water during the addition of the acid.
29. A process for preparing fexofenadine HCl comprising converting the fexofenadine free base of claim 12 to the HCl salt.
30. A process for preparing crystalline fexofenadine HCl salt comprising the steps of preparing a solution of fexofenadine keto acid in a water miscible organic solvent in the presence of a base and water; adding a reducing agent to the solution to reduce the keto-acid; acidifying reaction mixture obtained from the reduction to precipitate fexofenadine free base, recovering the crystalline form of fexofenadine free base and converting it HCl salt.
The claims below are in addition to those above.
All refrences to claim(s) which appear below refer to the numbering after this setence.
We claim:
1. A toner compositor, comprising:
resin particles;
pigment particles;
wax particles; and
an amount of a compatibilizing component effective to improve the homogeneity of the composition, where the compatibilizing component is a coupled alcohol ethoxylate.
2. The toner composition of claim 1 where the resin particles are selected from the group consisting of polyesters, copolyesters and mixtures thereof, reactively extruded polyesters, styrene butadiene copolymers, styrene acrylate copolymers, and styrene methacrylate copolymers.
3. The toner composition of claim 1 where the pigment particles are magnetic.
4. The toner composition of claim 1 where the pigment particles comprise carbon black and magnetites.
5. The toner composition of claim 1 where the pigment particles are selected from the group consisting of magenta, cyan, yellow and mixtures thereof.
6. The toner composition of claim 1 further comprising additional wax components, different from the wax particles, to improve fixrelease characteristics.
7. The toner composition of claim 1 where the compatibilizing component is the reaction product of an ethoxylated alcohol with a diisocyanate.
8. The toner composition of claim 7 where the diisocyanate is selected from the group consisting of toluene diisocyanate (TDI), methylenediphenyl diisocyanate (MDI), and mixtures thereof.
9. The toner composition of claim 1 where the compatibilizing component is the reaction product of an ethoxylated alcohol with an aromatic diisocyanate in an approximate ratio of from 0.2 to 1.5 equivalents of aromatic diisocyanate per OH equivalent of ethoxylated alcohol.
10. A powder coating comprising:
resin particles;
pigment particles;
wax particles;
extender particles; and
an amount of a compatibilizing component effective to improve the homogeneity of the composition, where the compatibilizing component is a coupled alcohol ethoxylate.
11. The powder coating of claim 10 further comprising a degassing agent.
12. The powder coating of claim 11 where the degassing agent is present in an amount of from about 0.05 percent to 20 about percent by weight based on the entire coating composition.
13. The powder coating of claim 10 where the resin particles are selected from the group consisting of polyester, epoxy, and acrylic and mixtures thereof.
14. The powder coating of claim 10 where the resin particles comprise polyester-hydroxyalkylamide powders.
15. The powder coating of claim 10 where the compatibilizing component is present in an amount of from about 0.05 percent to about 20 percent by weight based on the entire coating composition.
16. The powder coating of claim 10 where the compatibilizing component is the reaction product of an ethoxylated alcohol with a diisocyanate.
17. The powder coating of claim 16 where the diisocyanate is selected from the group consisting of toluene diisocyanate (TDI), methylenediphenyl diisocyanate (MDI), and mixtures thereof.
18. The powder coating of claim 10 where the compatibilizing component is the reaction product of an ethoxylated alcohol with an aromatic diisocyanate in an approximate ratio of from 0.2 to 1.5 equivalents of aromatic diisocyanate per OH equivalent of ethoxylated alcohol.
19. The powder coating of claim 10 where the wax particles are selected from the group consisting of non-reactive and reactive wax particles.
20. A polish (wax) for an article comprising an amount of a coupled alcohol ethoxylate effective to improve adhesion.
21. The polish of claim 20 where the coupled alcohol ethoxylate is the reaction product of an ethoxylated alcohol with a diisocyanate.
22. The polish of claim 21 where the diisocyanate is selected from the group consisting of toluene diisocyanate (TDI), methylenediphenyl diisocyanate (MDI), and mixtures thereof.
23. The polish of claim 20 where the coupled alcohol ethoxylate is the reaction product of an ethoxylated alcohol with an aromatic diisocyanate in an approximate ratio of from 0.2 to 1.5 equivalents of aromatic diisocyanate per OH equivalent of ethoxylated alcohol.
24. A coupled alcohol ethoxylate produced by the process comprising reacting an ethoxylated derivative of saturated linear alcohols having a carbon atom chain length ranging from about 20 to about 70 with a diisocyanate.
25. The coupled alcohol ethoxylate of claim 24 where the diisocyanate is selected from the group consisting of toluene diisocyanate (TDI), methylenediphenyl diisocyanate (MDI), and mixtures thereof.
26. The coupled alcohol ethoxylate of claim 24 where the coupled alcohol ethoxylate is the reaction product of an ethoxylated alcohol with an aromatic diisocyanate in an approximate ratio of from 0.2 to 1.5 equivalents of aromatic diisocyanate per OH equivalent of ethoxylated alcohol.