氯化铑(三水)置于triphenylphosphine,Formaldehyde,Sodium Ethoxide体系中,用 乙醇 用作溶剂,以75%的收率获得三(三苯基膦)羰基氢化铑 参考文献:The Crystal And Molecular Structure Of A New Polymorph Of Carbonylhydridotris(Triphenylphosphine)Rhodium(I) Having A Rh-H Stretching Absorption At 2013 Cm1 标题:The Crystal And Molecular Structure Of A New Polymorph Of Carbonylhydridotris(Triphenylphosphine)Rhodium(I) Having A Rh-H Stretching Absorption At 2013 Cm1 摘要:A New Polymorph Of Hrh(Co)(Pph(3)),,With A Upsilon Rh-H Of 2013 Cm(-1),Has Been Isolated By Crystallization From Tert-Butyl Methyl Ether/tetrahydrofuran. The Crystals Are Monoclinic (Space Group P2(I)/n),With A=21.48(2)Angstrom,B=14.92(2)Angstrom,C=14.52(1)Angstrom,Beta=107.95(8)Degrees. A Final R Value Of 0.065 Was Obtained Using 2243 Reflections Which Had I-Net>2.5 Sigma(I-Net). The Structure Of The New Polymorph Has A Similar Coordination Geometry To The Known Polymorph,But A Different Conformation Of One Of The Phenyl Rings. Doi:10.1007/bf01185550
专利信息
专利号:US-4668809-A 优先权日:1982-05-03 标 题 :Transition metal complex catalysts 发明人:OSWALD ALEXIS A; JERMASEN TORRIS G; WESTNER ANDREW A; HUANG I-DER 权利人:EXXON RESEARCH ENGINEERING CO 摘要:Compositions of matter are disclosed which are highly useful in hydroformylation processes. The compositions are non-charged, non-chelated bis- and tris-(alkyl diaryl phosphine) rhodium carbonyl hydrides. The substituents of the alkyl group includes heteroorganic radicals containing ether, ester, keto and hydroxy oxygen, phosphine oxide and phosphorus ester phosphorus, amine, amide, amine oxide and heterocyclic nitrogen groups. These compositions are highly stable and selective catalysts for the hydroformylation of olefins under certain conditions. The disclosed catalyst systems contain a large excess of phosphine ligand and employ alpha-olefin plus synthesis gas reactant mixtures having a high H2/CO ratio at relatively low pressures. They produce moslty aldehydes derived from terminal attack on the alpha-olefin reactant. In the case of low olefins, such as butene-1, the products can be advantageously removed in a continuous manner, as distillate components from a ligand reaction mixture kept at an elevated temperature and continuously fed by an appropriate mixture of the reactants.
专利号:US-4687866-A 优先权日:1980-02-12 标 题:Ligand exchange process for producing alkyl diaryl phosphine rhodium carbonyl hydrides 发明人:OSWALD ALEXIS A; JERMANSEN TORRIS G; WESTNER ANDREW A; HUANG I-DER 权利人:EXXON RESEARCH ENGINEERING CO 摘要:Compositions of matter are disclosed which are highly useful in hydroformylation processes. The compositions are non-charged, non-chelated bis- and tris-(alkyl diaryl phosphine) rhodium carbonyl hydrides. The substituents of the alkyl group include heteroorganic radicals containing silane, silicone, ether, ester, keto and hydroxy oxygen, phosphine oxide and phosphorus ester phosphorus, amine, amide, amine oxide and heterocyclic nitrogen groups. These compositions are highly stable and selective catalysts for the hydroformylation of olefins under certain conditions. The disclosed catalyst systems contain a large excess of phosphine ligand and employ alpha-olefin plus synthesis gas reactant mixtures having a high H2/CO ratio at relatively low pressures. They produce mostly aldehydes derived from terminal attack on the alpha-olefin reactant. In the case of low olefins, such as butene-1, the products can be advantageously removed in a continuous manner, as distillate components from a ligand reaction mixture kept at an elevated temperature and continuously fed by an appropriate mixture of the reactants.
专利号:US-4687874-A 优先权日:1980-02-12 标题 :Selective hydroformylation process using alkyl diaryl phosphine rhodium carbonyl hydride catalysts 发明人:OSWALD ALEXIS A; JERMANSEN TORRIS G; WESTNER ANDREW A; HUANG I-DER 权利人:EXXON RESEARCH ENGINEERING CO 摘要:Compositions of matter are disclosed which are highly useful in hydroformylation processes. The compositions are non-charged, non-chelated bis- and tris-(alkyl diaryl phosphine) rhodium carbonyl hydrides. The substituents of the alkyl group include heteroorganic radicals containing ether, ester, keto and hydroxy oxygen, phosphine oxide and phosphorus ester phosphorus, amine, amide, amine oxide and heterocyclic nitrogen groups. These compositions are highly stable and selective catalysts for the hydroformylation of olefins under certain conditions. The disclosed catalyst systems contain a large excess of phosphine ligand and employ alpha-olefin plus synthesis gas reactant mixtures having a high H2/CO ratio at relatively low pressures. They produce mostly aldehydes derived from terminal attack on the alpha-olefin reactant. In the case of low olefins, such as butene-1, the products can be advantageously removed in a continuous manner, as distillate components from a ligand reaction mixture kept at an elevated temperature and continuously fed by an appropriate mixture of the reactants.
专利号:US-4595753-A 优先权日:1982-05-03 标 题:Heterocycle-substituted alkyl diaryl phosphine rhodium caronyl hydride complex hydroformylation catalyst compositions 发明人:OSWALD ALEXIS A; JERMASEN TORRIS G; WESTNER ANDREW A; HUANG I-DER 权利人:EXXON RESEARCH ENGINEERING CO 摘要:Compositions of matter are disclosed which are highly useful in hydroformylation processes. The compositions are non-charged, non-chelated bis- and tris-(alkyl diaryl phosphine) rhodium carbonyl hydrides. The substituents of the alkyl group include heteroorganic radicals containing silane, silicone, ether, ester, keto and hydroxy oxygen, phosphine oxide and phosphorus ester phosphorus, amine, amide, amine oxide and heterocyclic nitrogen groups. These compositions are highly stable and selective catalysts for the hydroformylation of olefins under certain conditions. The disclosed catalyst systems contain a large excess of phosphine ligand and employ alpha-olefin plus synthesis gas reactant mixtures having a high H2/CO ratio at relatively low pressures. They produce mostly aldehydes derived from terminal attack on the alpha-olefin reactant. In the case of low olefins, such as butene-1, the products can be advantageously removed in a continuous manner, as distillate components from a ligand reaction mixture kept at an elevated temperature and continuously fed by an appropriate mixture of the reactants.