Claims
- 1. A method for preparing a cross-bridged macropolycycle comprising a series of steps of derivatizing cyclam or a particular acyclic tetraamine, wherein said series of steps is carried out using one solvent system.
- 2. A method according to claim 1 wherein said solvent system is an alcoholic solvent system.
- 3. A method according to claim 1 wherein said solvent system comprises from about 60% to 100% of a C1-C4 alcohol or mixtures thereof.
- 4. A method according to claim 1 wherein said solvent system is ethanol or mixtures of ethanol with water.
- 5. A method according to claim 1 wherein said series of steps are all carried out in one reaction vessel.
- 6. A method for preparing a cross-bridged macropolycycle comprising a series of steps of derivatizing cyclam or a particular acyclic tetraamine including a step of quaternizing an intermediate using a quaternizing agent, wherein said step is carried out using less than fifteen-fold of said quaternizing agent.
- 7. A method according to claim 6 wherein said step is carried out using less than ten-fold of said quaternizing agent.
- 8. A method according to claim 6 wherein said step is carried out using from five-fold to ten-fold of said quaternizing agent.
- 9. A method according to claim 8 wherein said quaternizing agent is selected from the group consisting of methyl iodide, methyl tosylate, and dimethyl sulfate.
- 10. A method for preparing a cross-bridged macropolycycle according to claim 1 comprising a series of steps of derivatizing cyclam or a particular acyclic tetraamine including a step of reducing a diquaternized intermediate, wherein said step is carried out using an amount less than fifteen-fold of reducing agent.
- 11. A method for preparing a cross-bridged macropolycycle comprising a series of steps of derivatizing cyclam or a particular acyclic tetraamine including a step of reducing a diquaternized intermediate, wherein said step is carried out using an amount of less than fifteen-fold of reducing agent.
- 12. A method according to claim 11 wherein said reducing agent is a non-catalytic reducing agent.
- 13. A method according to claim 12 wherein said reducing agent is a hydride compound.
- 14. A method according to claim 13 wherein said hydride compound is a borohydride.
- 15. A method according to claim 14 wherein said borohydride compound is selected from the group consisting of sodium borohydride and potassium borohydride.
- 16. A method according to claim 15 wherein said borohydride compound is potassium borohydride.
- 17. A method for preparing a cross-bridged macropolycycle, said method comprising derivatizing cyclam or a particular acyclic tetraamine by a series of steps including:
quaternizing an intermediate using a quaternizing agent, wherein said step is carried out using less than fifteen-fold of said quaternizing agent; and reducing a diquaternized intermediate, wherein said step is carried out using an amount of less than fifteen-fold of reducing agent; and wherein further said series of steps is carried out using one solvent system.
- 18. A method according to claim 17, carried out in the absence of any step of vacuum distilling an intermediate.
- 19. A method according to claim 17, carried out at or below 50° C.
- 20. A method according to claim 17, wherein said quaternization and reduction steps are carried out at the temperatures of from ambient temperature to 50° C.
- 21. A method according to claim 17 wherein all of said steps are carried out at concentrations of the reactants of 7% or higher in total of the sum of reactants plus solvent.
- 22. A method according to claim 17 wherein all of said steps are carried out at concentrations of the reactants exceeding 15% in total of the sum of reactants plus solvent.
- 23. A method according to claim 14 in which sodium ion is substantially absent.
- 24. A method for producing a complex of Mn and a cross-bridged macropolycyclic ligand, said method comprising reacting with manganous chloride a cross-bridged macropolycycle.
- 25. A method for producing a complex of Mn and a cross-bridged macropolycyclic ligand, said method comprising reacting a cross-bridged macropolycycle with MnCl2 which has been produced by an anhydrous reaction of manganese metal with a chlorinating agent.
- 26. A method according to claim 24, conducted in a nonaqueous solvent.
- 27. A method according to claim 25, conducted in a nonaqueous solvent.
- 28. A method for preparing a transition metal complex of a cross-bridged macropolycycle comprising a series of steps of
(A) forming a bisaminal from an acyclic amine; (B) forming a diquat derivative of said bisaminal; (C) reducing said diquat derivative; (D) separating reducting agent and solvent from the product of step (C) in one or more operations; (E) removing residual hydride from the product of (D); (F) isolating a cross-bridged tetraazamacrocycle product of steps (A)-(E); and metal complex useful as a catalyst in detergent compositions.
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority under 35 USC §120 to U.S. application Ser. No. 09/832,579, filed Apr. 11, 2001, which claims priority under 35 USC §120 to U.S. application Ser. No. 09/380,675, filed Sep. 7, 1999, (now issued U.S. Pat. No. 6,225,464 B1) which is an entry into the U.S. National Stage under 35 U.S.C. §371 of PCT International Application Serial No. PCT/IB98/00299, filed Mar. 6, 1998, which claims priority under PCT Article 8 and 35 U.S.C. §119(e) to U.S. Provisional Application Serial No. 60/039,920, filed Mar. 7, 1997, (now abandoned).
Provisional Applications (1)
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Number |
Date |
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60039920 |
Mar 1997 |
US |
Continuations (1)
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Number |
Date |
Country |
Parent |
09380675 |
Sep 1999 |
US |
Child |
09832579 |
Apr 2001 |
US |
Continuation in Parts (1)
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Number |
Date |
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Parent |
09832579 |
Apr 2001 |
US |
Child |
10142085 |
May 2002 |
US |