Claims
- 1. A method for preparing sodium or potassium tetrakis(pentafluorophenyl) borate compound from a pentafluorophenyl magnesium bromide comprising the steps of:
reacting the (pentafluorophenyl) magnesium bromide in an ether with a tris(pentafluorophenyl) borane in an aromatic hydrocarbon solvent to produce tetrakis(pentafluorophenyl) borate magnesium bromide; reacting the tetrakis(pentafluorophenyl) borate magnesium bromide with an aqueous solution of a halide selected from the group consisting of sodium chloride and potassium chloride to create an organic phase containing a product compound selected from the group consisting of tetrakis(pentafluorophenyl) borate sodium salt and tetrakis(pentafluorophenyl) borate potassium salt; separating the organic phase; and removing solvent from the organic phase to provide a substantially ether-free compound selected from the group consisting of sodium tetrakis(pentafluorophenyl) borate and potassium tetrakis(pentafluorophenyl) borate.
- 2. The method according to claim 1, wherein the product compound comprises less than about 5.0 weight percent ether.
- 3. The method according to claim 1, wherein the product compound comprises less than about 3.0 weight percent ether.
- 4. The method according to claim 1, wherein the product compound comprises less than about 1.0 weight percent ether.
- 5. The method according to claim 1 further comprising, after step (a), the step of removing the ether for recycling.
- 6. The method according to claim 1 wherein the aromatic hydrocarbon is selected from the group consisting of xylene, ethylbenzene, and toluene.
- 7. The method according to claim 3, wherein the aromatic hydrocarbon is toluene.
- 8. The method according to claim 1, wherein the (pentafluorophenyl)magnesium bromide is reacted with the tris(pentafluorophenyl) borane at a temperature of from about 20 to about 65° C.
- 9. The method according to claim 1, wherein (pentafluorophenyl)magnesium bromide is reacted in a mixture comprising ether and toluene.
- 10. The method according to claim 9, wherein the ether is first removed from the organic phase by distilling the organic phase until a temperature about equal to the boiling point of toluene at atmospheric pressure is achieved.
- 11. The method according to claim 1, wherein the solvent is removed from the organic phase by distilling the organic phase until a temperature of about 110° C. at atmospheric pressure is achieved.
- 12. A method for making an essentially ether-free trityl tetrakis(pentafluorophenyl) borate comprising the steps of:
providing a substantially ether-free compound selected from the group consisting of sodium tetrakis(pentafluorophenyl) borate and potassium tetrakis(pentafluorophenyl) borate; reacting the substantially ether-free compound with a trityl halide in a hydrocarbon liquid to form a slurry of trityl tetrakis(pentafluorophenyl)borate and a halide in a hydrocarbon liquid; separating the trityl tetrakis (pentafluorophenyl) borate and halide from the hydrocarbon liquid by a method selected from the group consisting of filtration and decantation; dissolving trityl tetrakis(pentafluorophenyl) borate in a halogenated solvent to form a solution, said halogenated solvent free of oxygen, nitrogen or other coordinating atoms; and removing the solvent from the trityl tetrakis(pentafluorophenyl) borate solution.
- 13. The method according to claim 12, further comprising, before the step of removing the solvent from the borate solution, the step of diluting the trityl tetrakis(pentafluorophenyl) borate solution in a hydrocarbon solvent having a higher boiling point than the halogenated solvent.
- 14. The method according to claim 13, further comprising the step of removing the halogenated solvent and the hydrocarbon solvent to provide ether-free trityl tetrakis(pentafluorophenyl) borate product.
- 15. The method according to claim 12, wherein the trityl halide is trityl chloride.
- 16. The method according to claim 15, wherein trityl chloride is provided in an amount of from about 1 mole equivalents to about 3 mole equivalents relative to the amount of tetrakis(pentafluorophenyl)borate present.
- 17. The method according to claim 12, wherein trityl chloride is provided in an amount of from about 1.05 mole equivalents to about 2 mole equivalents relative to the amount of tetrakis(pentafluorophenyl)borate present.
- 18. The method according to claim 12, wherein trityl chloride is provided in an amount of from about 1.1 mole equivalents to about 1.6 mole equivalents relative to the amount of tetrakis(pentafluorophenyl) borate present.
- 19. The method according to claim 12, wherein the halide is sodium chloride.
- 20. The method according to claim 13, wherein the hydrocarbon solvent comprises hydrocarbon compounds having six to ten carbon atoms.
- 21. The method according to claim 13, wherein the hydrocarbon solvent is heptane.
- 22. The method according to claim 12, wherein the halogenated solvent is selected from the group consisting of CH2Cl2, CHCl3, CCl4 and CF3CCl3.
- 23. The method according to claim 12, wherein the halogenated solvent further comprises a hydrocarbon solvent.
- 24. The method according to claim 12, wherein the halogenated solvent is methylene chloride.
- 25. The method according to claim 23, wherein the hydrocarbon solvent comprises hydrocarbon compounds having from 6 to 10 carbon atoms.
- 26. The method according to claim 23, wherein the hydrocarbon solvent is heptane.
- 27. The method according to claim 23, wherein the hydrocarbon solvent is non-aromatic.
- 28. The method according to claim 12, wherein the borate solution yields a product substantially free of inorganic salts.
- 29. The method according to claim 12 wherein the borate solution yields a product substantially free of polar solvents and contaminating compounds.
- 30. The method according to claim 13, wherein the borate solution yields a product yellow in color.
- 31. The method according to claim 12, wherein the borate solution yields trityl tetrakis(pentafluorophenyl)borate comprising less than about 0.5 weight percent ether.
- 32. The method according to claim 12, wherein the borate solution yields trityl tetrakis(pentafluorophenyl)borate comprising less than about 0.1 weight percent ether.
- 33. Trityl tetrakis (pentafluorophenyl)borate made according to the method of claim 12.
- 34. The trityl tetrakis (pentafluorophenyl)borate of claim 33, comprising less than about 0.5 weight percent ether.
- 35. The trityl tetrakis (pentafluorophenyl)borate of claim 33, comprising less than about 0.1 weight percent ether.
- 36. Solid, essentially ether-free trityl-tetrakis(pentafluorophenyl) borate.
- 37. The borate according to claim 36, comprising less than about 0.5 weight percent ether.
- 38. The borate according to claim 36, comprising less than about 0.3 weight percent ether.
- 39. The borate according to claim 36, comprising less than about 0.1 weight percent ether.
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 60/212,588, filed Jun. 19, 2000.
Provisional Applications (1)
|
Number |
Date |
Country |
|
60212588 |
Jun 2000 |
US |