| 主权项 |
1. A method for producing a diphosphite of Structure I,comprising the steps of:
contacting a phosphorochloridite of Structure II, with a bisaryl compound selected from the group consisting of Structure III, Structure IV, and Structure V, and a tertiary organic amine, comprising a basic nitrogen atom or a plurality of nitrogen atoms, to produce a reaction mixture comprising a diphosphite of Structure I and at least one phosphorus-containing co-product in the reaction mixture selected from the group consisting of P(OR1)(OR2)2, P(OR1)2(OR2), P(OR1)3, P(OR2)3, a compound of Structure VIa, and a compound of Structure VIb,wherein,
the contacting is done by at least one contacting method selected from the group consisting of,
(i). feeding the bisaryl compound to a mixture of phosphorochloridite and tertiary organic amine, and(ii). feeding the bisaryl compound and the tertiary organic amine separately or as a mixture to the phosphorochloridite; and the contacting step is carried out by controlling the feeding such that a first mole ratio is maintained at equal to or greater than 2.0 during at least an initial stage and a final stage of the contacting step, wherein the first mole ratio is defined as moles of phosphorochloridite in the reaction mixture divided by moles of bisaryl compound fed to the reaction mixture, and the contacting step is carried out by controlling the feeding such that a second mole ratio is at least 1.0 during the contacting step, wherein the second mole ratio is defined as moles of basic nitrogen atoms from the tertiary organic amine fed to the reaction mixture divided by moles of phosphorochloridite in the reaction mixture, wherein the contacting is performed at a temperature of the reaction mixture of from greater than 10° C. to less than or equal to about 110° C.; and the method is characterized by
(1) controlling the feeding such that the first mole ratio is from 2.1 to 2.7 during the stage of the contacting wherein phosphorochloridite conversion is from 90% to 100%; and(2) optionally, controlling the feeding such that a phosphorochloridite concentration is greater than or equal to 0.02 moles per liter in the reaction mixture during the stage of the contacting wherein phosphorochloridite conversion is from 0% to 90%;wherein,
less than 30% of the total phosphorus in the reaction mixture is in the form of the at least one phosphorus-containing co-product, and 7.9% or less of the total phosphorus in the reaction mixture is in the form of the phosphorus-containing co-products having Structures VIa and VIb,wherein in Structures I to V and the at least one phosphorus-containing co-product,
R1 and R2 are the same or different, substituted or unsubstituted, monovalent aryl groups; 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 halogenyl groups; and O-Q-O− is a dianion of the bisaryl compound. |
