Claims
- 1. A method for preparing a cross-bridged macropolycycle, said method comprising derivatizing N,N′-bis-(2-aminoethyl)-1,3-propanediamine 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 less than fifteen-fold of reducing agent; and wherein further said series of steps is carried out using one solvent system and in the absence of any step of vacuum distilling an intermediate.
- 2. A method according to claim 1, carried out at or below 50° C.
- 3. A method according to claim 1, wherein said quaternization and reduction steps are carried out at the temperatures of from ambient temperature to 50° C.
- 4. 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 prepared in accordance with claim 1.
- 5. A method for producing a complex of Mn and a cross-bridged macropolycyclic ligand, said method comprising reacting a cross-bridged macropolycycle prepared in accordance with claim 1 with MnCl2 which has been produced by an anhydrous reaction of manganese metal with a chlorinating agent.
- 6. A method according to claim 4, conducted in a nonaqueous solvent.
- 7. A method according to claim 5, conducted in a nonaqueous solvent.
CROSS REFERENCE TO RELATED APPLICATIONS
This is a continuation under 35 U.S.C. §120 of U.S. application Ser. No. 09/380,675, filed Sep. 7, 1999 now U.S. Pat. No. 6,225,464 of which in turn claims priority under 35 U.S.C. §371 to PCT International Application Serial No. PCT/IB98/00299, filed Mar. 6, 1998 which claims priority under 35 U.S.C. §119(e) to U.S. Provisional Application Serial No. 60/039,920, filed Mar. 7, 1997.
US Referenced Citations (1)
Number |
Name |
Date |
Kind |
6225464 |
Hiler, II et al. |
May 2001 |
B1 |
Non-Patent Literature Citations (2)
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Weisman et al J. Am. Chem. Soc. 112 (1990) 8604-8605.* |
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Provisional Applications (1)
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Number |
Date |
Country |
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60/039920 |
Mar 1997 |
US |
Continuations (1)
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Number |
Date |
Country |
Parent |
09/380675 |
|
US |
Child |
09/832579 |
|
US |