| 主权项 |
1. A method for producing a phosphorus-containing diphosphite ligand structure (DLS) having the chemical structure of Structure I,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 one or more compounds 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, the second serial addition comprising the determined amount of one or more compounds selected from the group consisting of the X—OH, water, and 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 the X—OH or of one or more compounds selected from the group consisting of water and the alcohol having the chemical structure R1—OH or R2—OH, to add in a third serial addition; andadding the third serial addition to the second reaction mixture, comprising the X—OH or one or more compounds selected from the group consisting of 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 the X—OH is a bisaryl compound selected from the group consisting of Structure III, Structure IV, and Structure V: wherein Q has a structure selected from the group consisting of: wherein the at least one side-product comprises a C-phite ligand structure (CLS), having the chemical structure shown below as Structure VI, VII, or VIII, wherein providing a pre-determined limit for the mole percent of phosphorus present as at least one side-product in the final reaction mixture comprises providing a pre-determined limit for a mole percent of phosphorus present as CLS in the final reaction mixture; wherein in Structures I-VIII, 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 R3, R4, R5, R6, R7, R8, R9, R10, R11, and R12 is independently selected from the group consisting of hydrogen, alkyl, aryl, heteroaryl, aryloxy, heteroaryloxy, alkyloxy, alkoxyalkyl, acetal, carboaryloxy, carboalkoxy, arylcarbonyl, alkylcarbonyl, oxazole, amine, amide, nitrile, mercaptyl, and halogen groups; wherein alkyl refers to straight chain (C1-C20)alkyl groups, branched (C1-C20)alkyl groups or (C3-C20)cycloalkyl groups. |
