Cyclization/Hydrosilylation of Functionalized 1,6-Diynes Catalyzed by Cationic Platinum Complexes Containing Bidentate Nitrogen Ligands

A 1:1 mixture of the platinum dimethyl diimine complex [PhNC(Me)C(Me)NPh]PtMe2 (4a) and B(C6F5)3 catalyzed the cyclization/hydrosilylation of dimethyl dipropargylmalonate (1) and HSiEt3 to form 1,1-dicarbomethoxy-3-methylene-4-(triethylsilylmethylene)cyclopentane (3) in 82% isolated yield with 26:...

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Published inJournal of organic chemistry Vol. 67; no. 9; pp. 2778 - 2788
Main Authors Wang, Xiang, Chakrapani, Harinath, Madine, James W, Keyerleber, Michele A, Widenhoefer, Ross A
Format Journal Article
LanguageEnglish
Published WASHINGTON American Chemical Society 03.05.2002
Amer Chemical Soc
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ISSN0022-3263
1520-6904
DOI10.1021/jo015986p

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Abstract A 1:1 mixture of the platinum dimethyl diimine complex [PhNC(Me)C(Me)NPh]PtMe2 (4a) and B(C6F5)3 catalyzed the cyclization/hydrosilylation of dimethyl dipropargylmalonate (1) and HSiEt3 to form 1,1-dicarbomethoxy-3-methylene-4-(triethylsilylmethylene)cyclopentane (3) in 82% isolated yield with 26:1 Z:E selectivity. Platinum-catalyzed diyne cyclization/hydrosilylation tolerated a range of functional groups including esters, sulfones, acetals, silyl ethers, amides, and hindered ketones. Diynes that possessed propargylic substitution underwent facile cyclization/hydrosilylation to form silylated 1,2-dialkylidene cyclopentanes as mixtures of regioisomers. Diynes that possessed an electron-deficient internal alkyne underwent cyclization/hydrosilylation in moderate yield to form products resulting from silyl transfer to the less substituted alkyne. The silylated 1,2-dialkylidenecyclopentanes formed via diyne cyclization/hydrosilylation underwent a range of transformations including protodesilylation, Z/E isomerization, and [4 + 2] cycloaddition with dieneophiles.
AbstractList A 1:1 mixture of the platinum dimethyl diimine complex [PhN[double bond]C(Me)C(Me)[double bond]NPh]PtMe(2) (4a) and B(C(6)F(5))(3) catalyzed the cyclization/hydrosilylation of dimethyl dipropargylmalonate (1) and HSiEt(3) to form 1,1-dicarbomethoxy-3-methylene-4-(triethylsilylmethylene)cyclopentane (3) in 82% isolated yield with 26:1 Z:E selectivity. Platinum-catalyzed diyne cyclization/hydrosilylation tolerated a range of functional groups including esters, sulfones, acetals, silyl ethers, amides, and hindered ketones. Diynes that possessed propargylic substitution underwent facile cyclization/hydrosilylation to form silylated 1,2-dialkylidene cyclopentanes as mixtures of regioisomers. Diynes that possessed an electron-deficient internal alkyne underwent cyclization/hydrosilylation in moderate yield to form products resulting from silyl transfer to the less substituted alkyne. The silylated 1,2-dialkylidenecyclopentanes formed via diyne cyclization/hydrosilylation underwent a range of transformations including protodesilylation, Z/E isomerization, and [4 + 2] cycloaddition with dieneophiles.A 1:1 mixture of the platinum dimethyl diimine complex [PhN[double bond]C(Me)C(Me)[double bond]NPh]PtMe(2) (4a) and B(C(6)F(5))(3) catalyzed the cyclization/hydrosilylation of dimethyl dipropargylmalonate (1) and HSiEt(3) to form 1,1-dicarbomethoxy-3-methylene-4-(triethylsilylmethylene)cyclopentane (3) in 82% isolated yield with 26:1 Z:E selectivity. Platinum-catalyzed diyne cyclization/hydrosilylation tolerated a range of functional groups including esters, sulfones, acetals, silyl ethers, amides, and hindered ketones. Diynes that possessed propargylic substitution underwent facile cyclization/hydrosilylation to form silylated 1,2-dialkylidene cyclopentanes as mixtures of regioisomers. Diynes that possessed an electron-deficient internal alkyne underwent cyclization/hydrosilylation in moderate yield to form products resulting from silyl transfer to the less substituted alkyne. The silylated 1,2-dialkylidenecyclopentanes formed via diyne cyclization/hydrosilylation underwent a range of transformations including protodesilylation, Z/E isomerization, and [4 + 2] cycloaddition with dieneophiles.
A 1:1 mixture of the platinum dimethyl diimine complex [PhNT=C(,Me)C(Me)=NPh]PtMe2 (4a) and B(C6F5)(3) catalyzed the cyclization/hydrosilylation of dimethyl dipropargylmalonate (1) and HSiEt3 to form 1,1-dicarbomethoxy-3-methylene-4-(triethylsilylmethylene)cyclopentane (3) in 82% isolated yield,with 26:1 Z:E selectivity. Platinum-catalyzed diyne cyclization/hydrosilylation tolerated a range of functional groups including esters, sulfones, acetals, silyl ethers, amides, and hindered ketones, Diynes that possessed propargylic substitution underwent facile cyclization/hydrosilylation to form silylated 1,2-dialkylidene cyclopentanes as mixtures of regioisomers. Diynes that possessed an electron-deficient internal alkyne underwent cyclization/hydrosilylation in moderate yield to form products resulting from silyl transfer to the less substituted alkyne. The silylated 1,2-dialkylidenecyclopentanes formed via diyne cyclization/hydrosilylation underwent a range of transformations including protodesilylation, Z/E isomerization, and [4 + 2] cycloaddition with dieneophiles.
A 1:1 mixture of the platinum dimethyl diimine complex [PhN[double bond]C(Me)C(Me)[double bond]NPh]PtMe(2) (4a) and B(C(6)F(5))(3) catalyzed the cyclization/hydrosilylation of dimethyl dipropargylmalonate (1) and HSiEt(3) to form 1,1-dicarbomethoxy-3-methylene-4-(triethylsilylmethylene)cyclopentane (3) in 82% isolated yield with 26:1 Z:E selectivity. Platinum-catalyzed diyne cyclization/hydrosilylation tolerated a range of functional groups including esters, sulfones, acetals, silyl ethers, amides, and hindered ketones. Diynes that possessed propargylic substitution underwent facile cyclization/hydrosilylation to form silylated 1,2-dialkylidene cyclopentanes as mixtures of regioisomers. Diynes that possessed an electron-deficient internal alkyne underwent cyclization/hydrosilylation in moderate yield to form products resulting from silyl transfer to the less substituted alkyne. The silylated 1,2-dialkylidenecyclopentanes formed via diyne cyclization/hydrosilylation underwent a range of transformations including protodesilylation, Z/E isomerization, and [4 + 2] cycloaddition with dieneophiles.
A 1:1 mixture of the platinum dimethyl diimine complex [PhNC(Me)C(Me)NPh]PtMe2 (4a) and B(C6F5)3 catalyzed the cyclization/hydrosilylation of dimethyl dipropargylmalonate (1) and HSiEt3 to form 1,1-dicarbomethoxy-3-methylene-4-(triethylsilylmethylene)cyclopentane (3) in 82% isolated yield with 26:1 Z:E selectivity. Platinum-catalyzed diyne cyclization/hydrosilylation tolerated a range of functional groups including esters, sulfones, acetals, silyl ethers, amides, and hindered ketones. Diynes that possessed propargylic substitution underwent facile cyclization/hydrosilylation to form silylated 1,2-dialkylidene cyclopentanes as mixtures of regioisomers. Diynes that possessed an electron-deficient internal alkyne underwent cyclization/hydrosilylation in moderate yield to form products resulting from silyl transfer to the less substituted alkyne. The silylated 1,2-dialkylidenecyclopentanes formed via diyne cyclization/hydrosilylation underwent a range of transformations including protodesilylation, Z/E isomerization, and [4 + 2] cycloaddition with dieneophiles.
Author Wang, Xiang
Madine, James W
Widenhoefer, Ross A
Keyerleber, Michele A
Chakrapani, Harinath
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  surname: Widenhoefer
  fullname: Widenhoefer, Ross A
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Issue 9
Keywords ALPHA-OLEFINS
BIS-DIENES
1,6-DIENES
PYRIDINE-OXAZOLINE COMPLEXES
PALLADIUM COMPLEX
PHENANTHROLINE COMPLEX
C-H ACTIVATION
MEDIATED TETRAENE CARBOCYCLIZATIONS
ENYNE COMPOUND
CYCLIZATION
Catalytic reaction
Transition element complexes
Sulfone
Platinum Organic compounds
Amides
Organic silane
Hydrosilylation
Dienic compound
Ketone
Platinum I Complexes
Acetal
Ester
Bidentate ligand
Cycloaddition
Cyclization
Platinoid Complexes
Transition metal Organic compounds
Diynic compound
Chemical synthesis
Cyclopentane derivatives
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SSID ssj0000555
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Snippet A 1:1 mixture of the platinum dimethyl diimine complex [PhNC(Me)C(Me)NPh]PtMe2 (4a) and B(C6F5)3 catalyzed the cyclization/hydrosilylation of dimethyl...
A 1:1 mixture of the platinum dimethyl diimine complex [PhNT=C(,Me)C(Me)=NPh]PtMe2 (4a) and B(C6F5)(3) catalyzed the cyclization/hydrosilylation of dimethyl...
A 1:1 mixture of the platinum dimethyl diimine complex [PhN[double bond]C(Me)C(Me)[double bond]NPh]PtMe(2) (4a) and B(C(6)F(5))(3) catalyzed the...
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SubjectTerms Alkynes - chemistry
Catalysis
Chemistry
Chemistry, Organic
Cyclization
Drug Design
Exact sciences and technology
Hydrocarbons, Cyclic - chemical synthesis
Magnetic Resonance Spectroscopy
Models, Molecular
Molecular Structure
Nitrogen - chemistry
Organic chemistry
Organometalloidal and organometallic compounds
Organoplatinum Compounds - chemistry
Oxidation-Reduction
Physical Sciences
Preparations and properties
Science & Technology
Si derivatives
Silanes - chemistry
Stereoisomerism
Title Cyclization/Hydrosilylation of Functionalized 1,6-Diynes Catalyzed by Cationic Platinum Complexes Containing Bidentate Nitrogen Ligands
URI http://dx.doi.org/10.1021/jo015986p
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https://www.ncbi.nlm.nih.gov/pubmed/11975528
https://www.proquest.com/docview/71628990
Volume 67
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