摘要:
It has been discovered that the meso form of metallocenes can be catalytically isomerized to the racemic form of the metallocene. This is accomplished by heating an isomerization mixture formed from (i) a meso form of a bridged metallocene or a mixture of meso and racemic forms of a bridged metallocene, (ii) a Group 1 and/or 2 metal halide isomerization catalyst, and (iii) a liquid organic isomerization medium, such that at least a portion of the meso form of the metallocene is isomerized to the racemic form.
摘要:
One aspect of the invention is a process for purifying a pentafluorophenyl boron compound from a crude mixture comprised of the pentafluorophenyl boron compound and impurities, the impurirtes at least comprised of an ether and water, the process comprising: (a) mixing the crude mixture with an azeotropic organic solvent which (i) is capable of azeotrope formation with the water and (ii) has a boiling point above the boiling point of the ether; (b) distilling the resulting solution to remove at least a portion of the impurities; and (c) cooling the distilled solution so that a precipitate comprised of the pentafluorophenyl boron compound is formed. Processes are also described for producing pentafluorophenyl boron compounds which are particularly pure, dry and fine.
摘要:
A palladium-catalyzed arylation of an olefin with aryl halide and/or substituted aryl halide is conducted in a liquid polar organic solvent, and (ii) secondary or tertiary amine that boils (1) below the boiling temperature of the solvent if only one solvent is used or (2) below the boiling temperature of at least one, but not necessarily all, of the solvents if more than one is used. With the reaction mixture so formed (which comprises olefinically-substituted aromatic compound, amine-hydrohalide and solvent) is mixed a concentrated aqueous solution of inorganic base having a base strength greater than the base strength of the amine. This converts amine-hydrohalide to free amine and alkali metal halide, and forms (i) an aqueous phase containing dissolved alkali metal halide, and (ii) an organic phase comprising olefinically-substituted aromatic compound, amine and solvent. After separating these phases, amine is distilled off from the organic phase under low temperature and pressure conditions that suppress thermal oligomerization of the olefinically-substituted aromatic compound contained in the organic phase. The organic phase, when substantially freed of amine, is subjected to a palladium-catalyzed carboxylation with carbon monoxide and water and/or alcohol. The relatively high specific gravity of the aqueous phase greatly facilitates the phase separation, and enables efficient recovery of amine and recycle of solvent.
摘要:
This invention relates to a method for converting calcium salts of [S,S]-ethylenediamine-N,N'-disuccinic acid to an easily filterable precipitate of [S,S]-ethylenediamine-N,N'-disuccinic acid comprising: co-feeding, to a volume of water, calcium [S,S]-ethylenediamine-N,N'-disuccinic acid salt and aqueous mineral acid, the mineral acid having a dissociation constant within the range of from about 1.0 x 10 to about 1.0 x 10 , wherein the feed rates of the calcium salt and the aqueous mineral acid are controlled so that the volume of water has a pH within the range of from about 1.4 to about 7 at least substantially throughout the co-feed period.
摘要:
Bromination of styrenic polymer is carried out in a closed reaction system to retain BK coproduct (where HX is HBr or HC1, or both) in the bromination reaction mixture at superatmospheric pressure. Preferably, the reaction mixture which includes the brominated styrenic polymer and substantially all of the HX coproduct formed is discharged into an aqueous quenching medium. By operating in this manner, the reaction is terminated and the brominated styrenic polymer of desired bromine content and substantially all HX coproduct are captured in the same operation, process equipment costs are reduced, and processing of the reaction mixture is facilitated.
摘要:
This invention relates to a process for selectively producing and recovering [S,S]-ethylenediamine-N,N'-disuccinic acid by the reaction of L-aspartic acid and 1,2-dihaloethane in an aqueous medium, wherein a stoichiometric deficiency of 1,2-dihaloethane is used and wherein the resultant aqueous solution obtained from the reaction is co-fed to water with a mineral acid to preferentially precipitate out [S,S]-ethylenediamine-N,N'-disuccinic acid from the solution.
摘要:
Bromination of styrenic polymer is carried out in a closed reaction system to retain BK coproduct (where HX is HBr or HC1, or both) in the bromination reaction mixture at superatmospheric pressure. Preferably, the reaction mixture which includes the brominated styrenic polymer and substantially all of the HX coproduct formed is discharged into an aqueous quenching medium. By operating in this manner, the reaction is terminated and the brominated styrenic polymer of desired bromine content and substantially all HX coproduct are captured in the same operation, process equipment costs are reduced, and processing of the reaction mixture is facilitated.
摘要:
One aspect of the invention is a process for purifying a pentafluorophenyl boron compound from a crude mixture comprised of the pentafluorophenyl boron compound and impurities, the impurirtes at least comprised of an ether and water, the process comprising: (a) mixing the crude mixture with an azeotropic organic solvent which (i) is capable of azeotrope formation with the water and (ii) has a boiling point above the boiling point of the ether; (b) distilling the resulting solution to remove at least a portion of the impurities; and (c) cooling the distilled solution so that a precipitate comprised of the pentafluorophenyl boron compound is formed. Processes are also described for producing pentafluorophenyl boron compounds which are particularly pure, dry and fine.
摘要:
Racemic, bridged hafnocene is produced in enhanced yield by reacting a hafnium halide-aliphatic polyether adduct that has been formed and/or heated at one or more temperatures of at least 40 °C, and a metallated bis(cyclopentadienyl-moiety-containing) ligand, at one or more temperatures for a sufficient period of time such that a racemic, bridged hafnocene is produced. The reaction is performed in the substantial absence of tetrahydrofuran and/or any other ether solvent or diluent that causes the formation of a tarry residue in the reaction mixture.