Convenient syntheses of [RuCl(CO)2(Cp)] and [OsCl(CO)2(Cp)]

Somanath Dev; John P. Selegue

doi:10.1016/0022-328X(94)80084-7

Convenient syntheses of [RuCl(CO)₂(Cp)] and [OsCl(CO)₂(Cp)]

Somanath Dev
, John P. Selegue

Producción científica: Article › revisión exhaustiva

18 Citas (Scopus)

Resumen

[RuCl(CO)₂(Cp)] (1) is obtained in two simple steps from [RuCl₃(H₂O)_x]. [RuCl₂(CO)₃]₂, produced by refluxing [RuCl₃(H₂O)_x] in hydrochloric and formic acids, reacts cleanly with [SiMe₃(C₅H₅)] to give [RuCl(CO)₂(Cp)] (1) in 74% overall yield from [RuCl₃(H₂O)_x]. [OsCl(CO)₂(Cp)] (2) is similarly obtained in four steps from [OsO₄]. Known conversion Of [OsO₄] to [NH₄]₂[OsCl₆], reduction to [OsCl₃] and carbonylation to [OsCl₂(CO)₃]₂ in a tube furnace, and finally reaction with [SiMe₃(C₅H₅)] give [OsCl(CO)₂(Cp)] (2) in 26% overall yield from [OsO₄]. These preparations are a significant improvement over previous published methods, avoiding the intermediacy of [M₃(CO)₁₂].

Idioma original	English
Páginas (desde-hasta)	107-110
Número de páginas	4
Publicación	Journal of Organometallic Chemistry
Volumen	469
N.º	1
DOI	https://doi.org/10.1016/0022-328X(94)80084-7
Estado	Published - abr 19 1994

Nota bibliográfica

Funding Information:
We are grateful to the US Departmento f Energy (DE-FGO5-85ER13432)a nd the Kentucky EPSCoR program( NSF Grant EHR-91-08764)f or financial support, the National ScienceF oundation(CHE-9113581) for equipment,a nd Johnson-Matthey,I nc., for a loan of rutheniumt richloride.W e thank Prof. Peter Eklund for the use of a tube furnace.

Financiación

We are grateful to the US Departmento f Energy (DE-FGO5-85ER13432)a nd the Kentucky EPSCoR program( NSF Grant EHR-91-08764)f or financial support, the National ScienceF oundation(CHE-9113581) for equipment,a nd Johnson-Matthey,I nc., for a loan of rutheniumt richloride.W e thank Prof. Peter Eklund for the use of a tube furnace.

Financiadores	Número del financiador
Kentucky-NSF EPSCoR Program
National ScienceF oundation	CHE-9113581
US Departmento f Energy	DE-FGO5-85ER13432
National Science Foundation (NSF)	EHR-91-08764

ASJC Scopus subject areas

Biochemistry
Physical and Theoretical Chemistry
Organic Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/0022-328X(94)80084-7

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title = "Convenient syntheses of [RuCl(CO)2(Cp)] and [OsCl(CO)2(Cp)]",

abstract = "[RuCl(CO)2(Cp)] (1) is obtained in two simple steps from [RuCl3(H2O)x]. [RuCl2(CO)3]2, produced by refluxing [RuCl3(H2O)x] in hydrochloric and formic acids, reacts cleanly with [SiMe3(C5H5)] to give [RuCl(CO)2(Cp)] (1) in 74\% overall yield from [RuCl3(H2O)x]. [OsCl(CO)2(Cp)] (2) is similarly obtained in four steps from [OsO4]. Known conversion Of [OsO4] to [NH4]2[OsCl6], reduction to [OsCl3] and carbonylation to [OsCl2(CO)3]2 in a tube furnace, and finally reaction with [SiMe3(C5H5)] give [OsCl(CO)2(Cp)] (2) in 26\% overall yield from [OsO4]. These preparations are a significant improvement over previous published methods, avoiding the intermediacy of [M3(CO)12].",

keywords = "Carbonyl, Chloride, Cyclopentadienyl, Nuclear magnetic resonance, Osmium, Ruthenium",

author = "Somanath Dev and Selegue, \{John P.\}",

note = "Funding Information: We are grateful to the US Departmento f Energy (DE-FGO5-85ER13432)a nd the Kentucky EPSCoR program( NSF Grant EHR-91-08764)f or financial support, the National ScienceF oundation(CHE-9113581) for equipment,a nd Johnson-Matthey,I nc., for a loan of rutheniumt richloride.W e thank Prof. Peter Eklund for the use of a tube furnace.",

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doi = "10.1016/0022-328X(94)80084-7",

language = "English",

volume = "469",

pages = "107--110",

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T1 - Convenient syntheses of [RuCl(CO)2(Cp)] and [OsCl(CO)2(Cp)]

AU - Dev, Somanath

AU - Selegue, John P.

N1 - Funding Information: We are grateful to the US Departmento f Energy (DE-FGO5-85ER13432)a nd the Kentucky EPSCoR program( NSF Grant EHR-91-08764)f or financial support, the National ScienceF oundation(CHE-9113581) for equipment,a nd Johnson-Matthey,I nc., for a loan of rutheniumt richloride.W e thank Prof. Peter Eklund for the use of a tube furnace.

PY - 1994/4/19

Y1 - 1994/4/19

N2 - [RuCl(CO)2(Cp)] (1) is obtained in two simple steps from [RuCl3(H2O)x]. [RuCl2(CO)3]2, produced by refluxing [RuCl3(H2O)x] in hydrochloric and formic acids, reacts cleanly with [SiMe3(C5H5)] to give [RuCl(CO)2(Cp)] (1) in 74% overall yield from [RuCl3(H2O)x]. [OsCl(CO)2(Cp)] (2) is similarly obtained in four steps from [OsO4]. Known conversion Of [OsO4] to [NH4]2[OsCl6], reduction to [OsCl3] and carbonylation to [OsCl2(CO)3]2 in a tube furnace, and finally reaction with [SiMe3(C5H5)] give [OsCl(CO)2(Cp)] (2) in 26% overall yield from [OsO4]. These preparations are a significant improvement over previous published methods, avoiding the intermediacy of [M3(CO)12].

AB - [RuCl(CO)2(Cp)] (1) is obtained in two simple steps from [RuCl3(H2O)x]. [RuCl2(CO)3]2, produced by refluxing [RuCl3(H2O)x] in hydrochloric and formic acids, reacts cleanly with [SiMe3(C5H5)] to give [RuCl(CO)2(Cp)] (1) in 74% overall yield from [RuCl3(H2O)x]. [OsCl(CO)2(Cp)] (2) is similarly obtained in four steps from [OsO4]. Known conversion Of [OsO4] to [NH4]2[OsCl6], reduction to [OsCl3] and carbonylation to [OsCl2(CO)3]2 in a tube furnace, and finally reaction with [SiMe3(C5H5)] give [OsCl(CO)2(Cp)] (2) in 26% overall yield from [OsO4]. These preparations are a significant improvement over previous published methods, avoiding the intermediacy of [M3(CO)12].

KW - Carbonyl

KW - Chloride

KW - Cyclopentadienyl

KW - Nuclear magnetic resonance

KW - Osmium

KW - Ruthenium

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