Anionic initiated coupling of tungsten carbene complexes: synthesis of the first (μ-tris(carbene))trimetallic complex

David W. Macomber; Mu Huang Hung

doi:10.1016/0022-328X(89)87323-1

Anionic initiated coupling of tungsten carbene complexes: synthesis of the first (μ-tris(carbene))trimetallic complex

David W. Macomber, Mu Huang Hung

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Abstract

Treatment of (CO)₅W[C(OCH₃)C(CH₃CH₂] (1) with C₂H₅(CH₃)₂CONa in THF at -78°C followed by HCl produced: (CO)₅W[C(OCH₃)CH(CH₃)CH₂OC(CH₃)₂C₂H₅] (3) (1%), C₂H₅(CH₃)₂CO(CO)₅W[C(OCH₃)C(CH₃)CH₂]CH₂C(CH₃)CH(OCH₃) (5) (<1%), C₂H₅(CH₃)₂CO (CO)₅W[C(OCH₃)C(CH₃)CH₂]₂H (6) (<1%), and the (μ-tris(carbene))trimetallic complex C₂H₅(CH₃)₂CO(CO)₅W[C(OCH₃)C(CH₃)CH₂]₃CH₂C(CH₃)CH(OCH₃) (9) (15%) as well as several, as yet, unidentified compounds. Complex 9 was characterized by analytical and spectroscopic methods; moreover, it was converted to the corresponding triester (10) upon PDC/DMSO oxidation. Upon standing at 0°C for long periods complex 1 was converted into a new (μ-bis(carbene))ditungsten complex (CO)₅WC(OCH₃)[CH(CH₃)CH₂CH₂C(CH₂)]C(OCH₃)W(CO)₅ (11) in low yield.

Original language	English (US)
Pages (from-to)	147-154
Number of pages	8
Journal	Journal of Organometallic Chemistry
Volume	366
Issue number	1-2
DOIs	https://doi.org/10.1016/0022-328X(89)87323-1
State	Published - Apr 25 1989
Externally published	Yes

Bibliographical note

Funding Information:
We wish to thank the Bureau of General Research (Kansas State University) for support of this research. High resolution mass spectra were performed by the Midwest Center for Mass Spectroscopy, a National Science Foundation Regional Instrumentation Facility (Grant No. CHE 8211164).

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title = "Anionic initiated coupling of tungsten carbene complexes: synthesis of the first (μ-tris(carbene))trimetallic complex",

abstract = "Treatment of (CO)5W[C(OCH3)C(CH3CH2] (1) with C2H5(CH3)2CONa in THF at -78°C followed by HCl produced: (CO)5W[C(OCH3)CH(CH3)CH2OC(CH3)2C2H5] (3) (1%), C2H5(CH3)2CO(CO)5W[C(OCH3)C(CH3)CH2]CH2C(CH3)CH(OCH3) (5) (<1%), C2H5(CH3)2CO (CO)5W[C(OCH3)C(CH3)CH2]2H (6) (<1%), and the (μ-tris(carbene))trimetallic complex C2H5(CH3)2CO(CO)5W[C(OCH3)C(CH3)CH2]3CH2C(CH3)CH(OCH3) (9) (15%) as well as several, as yet, unidentified compounds. Complex 9 was characterized by analytical and spectroscopic methods; moreover, it was converted to the corresponding triester (10) upon PDC/DMSO oxidation. Upon standing at 0°C for long periods complex 1 was converted into a new (μ-bis(carbene))ditungsten complex (CO)5WC(OCH3)[CH(CH3)CH2CH2C(CH2)]C(OCH3)W(CO)5 (11) in low yield.",

author = "Macomber, {David W.} and Hung, {Mu Huang}",

note = "Funding Information: We wish to thank the Bureau of General Research (Kansas State University) for support of this research. High resolution mass spectra were performed by the Midwest Center for Mass Spectroscopy, a National Science Foundation Regional Instrumentation Facility (Grant No. CHE 8211164).",

year = "1989",

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doi = "10.1016/0022-328X(89)87323-1",

language = "English (US)",

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T2 - synthesis of the first (μ-tris(carbene))trimetallic complex

AU - Macomber, David W.

AU - Hung, Mu Huang

N1 - Funding Information: We wish to thank the Bureau of General Research (Kansas State University) for support of this research. High resolution mass spectra were performed by the Midwest Center for Mass Spectroscopy, a National Science Foundation Regional Instrumentation Facility (Grant No. CHE 8211164).

PY - 1989/4/25

Y1 - 1989/4/25

N2 - Treatment of (CO)5W[C(OCH3)C(CH3CH2] (1) with C2H5(CH3)2CONa in THF at -78°C followed by HCl produced: (CO)5W[C(OCH3)CH(CH3)CH2OC(CH3)2C2H5] (3) (1%), C2H5(CH3)2CO(CO)5W[C(OCH3)C(CH3)CH2]CH2C(CH3)CH(OCH3) (5) (<1%), C2H5(CH3)2CO (CO)5W[C(OCH3)C(CH3)CH2]2H (6) (<1%), and the (μ-tris(carbene))trimetallic complex C2H5(CH3)2CO(CO)5W[C(OCH3)C(CH3)CH2]3CH2C(CH3)CH(OCH3) (9) (15%) as well as several, as yet, unidentified compounds. Complex 9 was characterized by analytical and spectroscopic methods; moreover, it was converted to the corresponding triester (10) upon PDC/DMSO oxidation. Upon standing at 0°C for long periods complex 1 was converted into a new (μ-bis(carbene))ditungsten complex (CO)5WC(OCH3)[CH(CH3)CH2CH2C(CH2)]C(OCH3)W(CO)5 (11) in low yield.

AB - Treatment of (CO)5W[C(OCH3)C(CH3CH2] (1) with C2H5(CH3)2CONa in THF at -78°C followed by HCl produced: (CO)5W[C(OCH3)CH(CH3)CH2OC(CH3)2C2H5] (3) (1%), C2H5(CH3)2CO(CO)5W[C(OCH3)C(CH3)CH2]CH2C(CH3)CH(OCH3) (5) (<1%), C2H5(CH3)2CO (CO)5W[C(OCH3)C(CH3)CH2]2H (6) (<1%), and the (μ-tris(carbene))trimetallic complex C2H5(CH3)2CO(CO)5W[C(OCH3)C(CH3)CH2]3CH2C(CH3)CH(OCH3) (9) (15%) as well as several, as yet, unidentified compounds. Complex 9 was characterized by analytical and spectroscopic methods; moreover, it was converted to the corresponding triester (10) upon PDC/DMSO oxidation. Upon standing at 0°C for long periods complex 1 was converted into a new (μ-bis(carbene))ditungsten complex (CO)5WC(OCH3)[CH(CH3)CH2CH2C(CH2)]C(OCH3)W(CO)5 (11) in low yield.

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ER -

Anionic initiated coupling of tungsten carbene complexes: synthesis of the first (μ-tris(carbene))trimetallic complex

Abstract

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