Methods of making cross-bridged macropolycycles
OwnerGeorge Douglas Hiler II, Christopher Mark Perkinsinventors
Life of this patent
Estimating the term…
Abstract
Improved synthesis of a macropolycycle, more particularly, of a cross-bridged tetraazamacrocycle.
Claims28
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.
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.
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.
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.
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.
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.
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.
Dependencies are inferred from the claim text.