主权项 |
1. A method for producing a phosphorus-containing ligand structure having the following chemical structure comprising:
contacting a phosphorochloridite of the following structure, with a compound having the chemical structure X—OH and a tertiary organic amine to provide a final reaction mixture comprising the ligand structure;
wherein the contacting comprises
providing a pre-determined limit for a mole percent of phosphorus present as at least one side-product in the final reaction mixture;adding the X—OH to the phosphorochloridite in a first serial addition, to provide a first reaction mixture;determining a mole percent of phosphorus present in the first reaction mixture as the at least one side-product;using a comparison of the mole percent of phosphorus present in the first reaction mixture as the at least one side-product to the pre-determined limit for the mole percent of phosphorus present as the at least one side-product in the final reaction mixture, to determine an amount of a compound selected from the group consisting of the X—OH, water, and an alcohol having the chemical structure R1—OH or R2—OH, to add in a second serial addition;adding the second serial addition to the first reaction mixture, comprising a compound selected from the group consisting of the X—OH, water, or the alcohol having the chemical structure R1—OH or R2—OH, to provide a second reaction mixture; andeither
performing third addition steps comprising optionally determining a mole percent of phosphorus present in the second reaction mixture as the at least one side-product; optionally using a comparison of the mole percent of phosphorus present in the second reaction mixture as the at least one side-product to the pre-determined limit for the mole percent of phosphorus present as the at least one side-product in the final reaction mixture, to determine an amount of a compound selected from the group consisting of the X—OH, water, and the alcohol having the chemical structure R1—OH or R2—OH, to add in a third serial addition; and adding the third serial addition to the second reaction mixture, comprising a compound selected from the group consisting of the X—OH, water, and the alcohol having the chemical structure R1—OH or R2—OH, to provide the final reaction mixture;or
the final reaction mixture is the second reaction mixture;wherein in Structures I′ and II, R1 and R2 are the same or different, substituted or unsubstituted, monovalent aryl groups; R1 and R2 are bridged to one another or unbridged to one another; and each of X and X′ are independently selected from the group consisting of hydrogen, alkyl, aryl, heteroaryl, aryloxy, heteroaryloxy, alkyloxy, alkoxyalkyl, acetal, carboaryloxy, carboalkoxy, arylcarbonyl, alkylcarbonyl, phosphitylbisaryl, phosphitylbisheteroaryl, hydroxybisaryl, hydroxybisheteroaryl, oxazole, amine, amide, nitrile, mercaptyl, and halogen groups. |