Chemie polyfunktioneller Liganden, 64 [1]. Über Hydridoiridium(III)-Komplexe des N.N-Bis(diphenylphosphino)-p-tolylamiii Chemistry of Polyfunctional Ligands, 64 [1]. On Hydridoiridium(III) Complexes of N,N-Bis(diphenylphosphino)-p-tolylamine

1981 ◽  
Vol 36 (5) ◽  
pp. 571-577 ◽  
Author(s):  
Jochen Ellermann ◽  
Leo Mader ◽  
Kurt Geibel
Keyword(s):  
Nmr Spectra ◽  
Oxidative Addition ◽  
H Nmr ◽  
New Compounds

H2 reacts with [Ir{(Ph2P)2N-p-C6H4CH3}2]Cl · 3 C6H6 (1) to give cis-[Ir(H)2{(Ph2P)2N-p-C6H4CH3}2]Cl · CH2Cl2 (2a). By reaction of 2a with NaBPh4 cis-[Ir(H)2{(Ph2P)2N-p-C6H4CH3}2]BPh4 (2 b) is obtained. Refluxing of 2a in CH2Cl2 yields trans-[lr(H)2{(Ph2P)2N-p-C6H4CH3}2]Cl · 1/2 CH2Cl2 (3a), which undegoes metatheses with NaBPh4 to trans-[Ir(H)2{(Ph2P)2N-p-C6H4CH3}2]BPh4 (3b). 3a is also formed by refluxing of 1 in methanol in the presence of oxygen. Oxidative addition of HCl to 1 and reaction with NaBPh4 yields trans-[Ir(H)(Cl){(Ph2P)2N-p-C6H4CH3}2]BPh4 (4b). The new compounds are characterised by their IR, Raman, 31P{1H} PFT and 1H NMR Spectra

scholarly journals New Synthetic Routes for 1-Benzyl-1,4,7,10-tetraazacyclododecane and 1,4,7,10-Tetraazacyclododecane-1-acetic Acid Ethyl Ester, Important Starting Materials for Metal-coded DOTA-Based Affinity Tags

2007 ◽  
Vol 62 (3) ◽  
pp. 397-406 ◽  
Author(s):  
Stephan W. Kohl ◽  
Katharina Kuse ◽  
Markus Hummert ◽  
Herbert Schumann ◽  
Clemens Mügge ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Ethyl Ester ◽  
Nmr Spectra ◽  
Acid Ethyl Ester ◽  
Affinity Tags ◽  
X Ray ◽  
H Nmr ◽  
Synthetic Routes ◽  
New Compounds ◽  
C Nmr

Two improved routes to synthesize 1-benzyl-1,4,7,10-tetraazacyclododecane (6) and 1,4,7,10- tetraazacyclododecane-1-acetic acid ethyl ester (11) are described as well as the synthesis of 1-{2-[4-(maleimido-N-propylacetamidobutyl)amino]-2-oxoethyl}-1,4,7,10-tetraazacyclododecane- 4,7,10-triacetic acid (17) and its Y, Ho, Tm, and Lu complexes. The 1H and 13C NMR spectra of the new compounds as well as the single crystal X-ray structure analyses of the intermediates 4-benzyl-1,7-bis(p-toluenesulfonyl)diethylenetriamine (3) and 1,4,7-tris(p-toluenesulfonyl)diethylenetriamine (7) are reported and discussed. The rare earth complexes of 17 have been characterized by 1H NMR spectroscopy and MALDI-TOF mass spectrometry.

Synthese und Eigenschaften von Alkyloxi-und Aryloxi-substituierten Trithiadiborolanen / Synthesis and Properties of Alkoxi and Aryloxi Substituted Trithiadiborolanes

1981 ◽  
Vol 36 (11) ◽  
pp. 1444-1450 ◽  
Author(s):  
Max Schmidt ◽  
Erich Sametschek
Keyword(s):  
Thermal Stability ◽  
Nmr Spectra ◽  
Chemical Properties ◽  
Physical And Chemical Properties ◽  
H Nmr ◽  
New Compounds ◽  
Physical And Chemical ◽  
Thermal Stability Of ◽  
And Chemical Properties

Abstract The first examples of the hitherto unknown 1,2,4-Trithia-3,5-diborolanes with B-O-C-bonds have been synthesized and characterised. The diiodo substituted ring (2) reacts with 2,6-dimethylphenol, to form 3,5-bis-(2,6-dimethylphenyloxi)-1,2,4-trithia-3,5-di-borolane (3) and HI. 3,5-Diethoxi-1,2,4-trithia-3,5-diborolane, 5, and C2H5I are formed via the cleavage of diethylether by 2. From 2 and diisopropylether, the corresponding 3,5-diisopropyloxi-1,2,4-trithia-3,5-diborolane (6) is formed. The unsymmetrical ethers methyl-t-butylether and methylphenylether undergo reactions with 2 resulting in the formation of 3,5-dimethyloxi-1,2,4-trithia-3,5-diborolane (8) (besides t-C4H9I) and 3,5-diphenyloxi-1,2,4-trithia-3,5-diborolane (10) (besides CH3I). The thermal stability of the new compounds is increasing with increasing size of R in the -OR group and from aliphatic to aromatic R in this group. IR, Raman, 1H NMR and 11B NMR spectra of the compounds are reported as well as some physical and chemical properties.

scholarly journals Komplexchemie polyfunktioneller Liganden, 52 [1]. Hydrido- und Deuterido-mangan(I)-carbonyl-Komplexe des 1.1.1- Tris (diphenylphosphinomeihy 1) ethans / Complex Chemistry of Polyfiinctional Ligands, 52 [1]. Hydrido- and Deuterido-manganese(I)-carbonyl Complexes of 1,1,1 -Tris(diphenylphosphinomethyl)ethane

1979 ◽  
Vol 34 (6) ◽  
pp. 799-804 ◽  
Author(s):  
Jochen Eilermann ◽  
Helmut A. Lindner
Keyword(s):  
Uv Irradiation ◽  
Methyl Alcohol ◽  
Ultraviolet Irradiation ◽  
Nmr Spectra ◽  
Carbonyl Complexes ◽  
Decomposition Products ◽  
H Nmr ◽  
Acetone Water ◽  
Complex Chemistry ◽  
New Compounds

[Mn(CO)3(R2PCH2)3CCH3]ClO4 (1a) (R = C6H5) reacts with NaBH4 on UV irradiation to yield HMn(CO)2(R2PCH2)3CCH3 (2a). [Mn(CO)3(R2PCH2)3CCH3]BR4 (1b) gives only decomposition products. Boiling of 1a or b and NaOH in acetone/water does nots give 2a but the new hydride HMn(CO)3(R2PCH2)2C(CH3)CH2PR2 (3a). This compound cannot be prepared on ultraviolet irradiation of a solution of 1a or b and NaBH4 in methyl alcohol or acetone. The analogous deutendes DMn(CO)2(R2)PCH2)3CCH3 (2b) and DMn(CO)3(R2PCH2)2C(CH3)CH2PR2 (3b) were also prepared. The new compounds were characterized by their IR, Raman, 1H NMR and 31P NMR spectra.

1,1,2,3,4,5 - Hexahydro Tellurophene [C4H8Te(II)] and 1,3-Dihydro-2λ4-Benzotellurole [C8H8Te(II)] Derivatives

2015 ◽  
Vol 7 (1) ◽  
Author(s):  
Rajesh Kumar ◽  
Sangeeta Bajpai
Keyword(s):  
Spectral Data ◽  
Elemental Analysis ◽  
Nmr Spectra ◽  
Oxidative Addition ◽  
Addition Reactions ◽  
Tellurium Atom ◽  
Oxidation Number ◽  
H Nmr ◽  
Data Table ◽  
Convenient Route

Convenient route of synthesis of the type R<sub>2</sub>TeX′SY and R<sub>2</sub>Te(CH<sub>3</sub>)X′c were dove loved by the reactions of R<sub>2</sub>Te(II) [R<sub>2</sub> = C<sub>4</sub>H<sub>8</sub>, C<sub>8</sub>H<sub>8</sub>] with IX′S (X′S= Cl, Br), RI (R = CH<sub>3</sub>, C<sub>2</sub>H<sub>5</sub>) and CH<sub>3</sub>X″c (X″c = Cl, Br, NO<sub>3</sub>, C<sub>6</sub>H<sub>5</sub>OCO).These complexes have been characterised through elemental analysis (Table 1) and <sup>1</sup>H NMR spectral data (Table 2). The <sup>1</sup>H NMR spectra of C<sub>4</sub>H<sub>8</sub>TeICl, C<sub>4</sub>H<sub>8</sub>TeIBr, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>I, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>Cl, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>Br, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>NO<sub>3</sub>, C<sub>4</sub>H<sub>8</sub>TeCH<sub>3</sub>OCOC<sub>6</sub>H<sub>5</sub>, C<sub>8</sub>H<sub>8</sub>TeCH<sub>3</sub>I, and C<sub>8</sub>H<sub>8</sub>Te -C<sub>2</sub>H<sub>5</sub>I have been recorded in CDCl<sub>3</sub> at 300 MHz. The study indicates that the heterocycles of C<sub>4</sub>H<sub>8</sub>Te(II) and C<sub>8</sub>H<sub>8</sub>Te(II) undergo oxidative addition reactions readily resulting in the increase in the oxidation number of central tellurium atom.

Sterische Wechselwirkungen im Innern cyclisdier Verbindungen, 19 / Steric Interactions of Inner Atoms in Cyclic Compounds, 191

1971 ◽  
Vol 26 (9) ◽  
pp. 872-874 ◽  
Author(s):  
Fritz Vögtle ◽  
Rainer Lichtenthaler
Keyword(s):  
Nmr Spectra ◽  
Conformational Mobility ◽  
Steric Interactions ◽  
H Nmr ◽  
Cyclic Compounds ◽  
New Compounds

The synthesis of a series of new heterocyclic [3.3] metacyclophanes has been carried out. The 1H-NMR-spectra of the new compounds have been studied with regard to configurational problems and conformational mobility.

Oxidative Addition Reactions of P(CN)3, P(NCO)3 and P(NCS)3 to (η5-C5Me5)Co(CO)2

1984 ◽  
Vol 39 (2) ◽  
pp. 142-144 ◽  
Author(s):  
S. Delgado ◽  
J. Macazaga ◽  
J. R. Masaguer
Keyword(s):  
Elemental Analysis ◽  
Nmr Spectra ◽  
Oxidative Addition ◽  
Addition Reactions ◽  
H Nmr

The phosphorus pseudohalogens P(CN)3, P(NCO)3 and P(NCS)3 react with (η5-C5Me5)Co(CO)2 to give the complexes (η5-C5Me5)Co(CO)XPX2 (X = CN, NCO, NCS). All the compounds are characterized by elemental analysis, IR. electronic and 1H NMR spectra

Preparation and polymerization of 3-(2-adamantyl)-3-methyl-2-azetidinone

1985 ◽  
Vol 50 (2) ◽  
pp. 454-458
Author(s):  
Jan Hauer ◽  
Jan Šebenda
Keyword(s):  
Melting Temperature ◽  
Intrinsic Viscosity ◽  
Anionic Polymerization ◽  
Nmr Spectra ◽  
H Nmr ◽  
New Compounds

3-(2-Adamantyl)-3-methyl-2-azetidinone (VI) was prepared, and new compounds, namely, methyl 2-(2-adamantyl) cyanoacetate, methyl-2-(2-adamantyl)-2-cyanopropanoate and methyl-2-(2-adamantyl)-2-methyl-3-aminopropanoate, were prepared in the course of the synthesis as intermediates. The anionic polymerization of lactam VI gave a polymer which was characterized by intrinsic viscosity, solubility, melting temperature and its IR and 1H NMR spectra. Compared with 3-butyl-3-methyl-2-azetidinone, lactam VI polymerizes much more slowly.

Diels-Alder Reactions of [1]Benzothieno[3,2-b]furan

1998 ◽  
Vol 63 (5) ◽  
pp. 681-697 ◽  
Author(s):  
Pavel Pihera ◽  
Jaroslav Paleček ◽  
Jiří Svoboda
Keyword(s):  
Nmr Spectra ◽  
Diels Alder ◽  
H Nmr ◽  
New Compounds

[1]Benzothieno[3,2-b]furan reacts with substituted dienes 2 as a dienophile under formation of substituted tetrahydro[1]benzothieno[3,2-b][1]benzofuran derivatives 3-14. The cycloaddition is endo-stereoselective. Aromatization of the products leads to a series of new fused [1]benzothieno[3,2-b][1]benzofurans 17-24. The 1H NMR spectra of the new compounds were fully assigned.

Chemie polyfunktioneller Liganden, 57 [1] Über Iridium(I)- und Platin(II)-Komplexe des Bis(diphenylphosphino)amins und die oxidative Addition kleiner Moleküle an Di[bis(diphenylphosphino)amin-P.P']iricUum(I)-chlorid / Chemistry of Polyfunctional Ligands, 57[1] About Iridium(I) and Platinum(II) Complexes of Bis(diphenylphosphino)amine and the Oxidative Addition of Small Molecules to Di[bis(diphenylphosphino)amine]iridium(I)-chloride

1980 ◽  
Vol 35 (3) ◽  
pp. 307-315 ◽  
Author(s):  
Jochen Ellermann ◽  
Leo Mader
Keyword(s):  
Small Molecules ◽  
Nmr Spectra ◽  
Oxidative Addition ◽  
Molar Ratio ◽  
Ionic Complex ◽  
Oxidative Additions ◽  
Square Planar ◽  
Deuterated Derivative ◽  
New Compounds

R2PNHPR2 (1) (R = C6H5) reacts with [(μ-Cl)Ir(C8H12)]2 in a molar ratio of 4:1, to give the square planar, ionic complex [Ir(R2PNHPR2)2]Cl (2a). By reaction of 2a with NaBR4, [Ir(R2PNHPR2)2]BR4 (2b) is obtained. Treatment of 2 a with CO gives [Ir(CO)(R2PNHPR2)2]Cl (3a). The complex 3a is also formed by the reaction of 1 with Ir(CO)(PR3)2Cl (R = C6H5) and Ir(CO)2(p-H2N-C6H4-CH3)Cl. 3a undergoes metathesis with NH4PF6 to yield [Ir(CO)(R2PNHPR2)2]PF6 (3b). The N-deuterated derivative [Ir(CO)(R2PNDPR2)2]Cl (4) is made by H/D exchange from 3a with CH3OD. Oxidative additions of O2 , CS2, I2 and (SCN)2 to 2a yield [Ir(O2)(R2PNHPR2)2]Cl (5), [Ir(μ2-CS2)(R2PNHPR2)2]Cl (6), [Ir(I)2(R2PNHPR2)2]Cl (7) and [Ir(SCN)2(R2PNHPR2)2]Cl (8). Additionally K2[PtCl4] and 1 reacts to [Pt(R2PNHPR2)2]Cl2 (9). The new compounds are characterised, as far as possible, by their IR, FIR, Raman and 31P NMR spectra.

Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, XLIX [1]. Untersuchungen zur Chelat-assistierten oxidativen Addition einer C–Cl-Bindung an Rhodium(I)-KompIexe und reaktives Verhalten von Phospha-rhoda-cyclopentanen / Preparation and Properties of, and Reactions with Metal-Containing Heterocycles, XLIX [1]. Investigations on the Chelate Assisted Oxidative Addition of a C–Cl Bond to Rhodium Complexes and Reactive Behaviour of Phospharhodacyclopentanes

1985 ◽  
Vol 40 (10) ◽  
pp. 1333-1337 ◽  
Author(s):  
Ekkehard Lindner ◽  
Riad Fawzi ◽  
Hermann August Mayer
Keyword(s):  
Electron Density ◽  
Nmr Spectra ◽  
Oxidative Addition ◽  
Rhodium Complexes ◽  
High Electron ◽  
High Electron Density ◽  
Free Rotation ◽  
Temperature Dependent ◽  
Triclinic Space Group ◽  
H Nmr

The complex L2Rh(CO)Cl (3b) is obtained by reaction of [μ-ClRh(CO)2)2 (1) with L = Cl-[CH2]3-P(C6H11)2 (2b) in benzene at 20 °C. 3b crystallizes in the triclinic space group P1 with Z = 1. On re fluxing 3 b in benzene an oxidative addition of one C-Cl bond to rhodium takes place to give the rhodacyclopentane derivative [xxx] (4b). Not only steric aspects of the ligands L and high electron density of the metal, but also free rotation about the Rh-P axis is important for the oxidative addition. Temperature dependent 31P{1H} NMR spectra of 3b between - 90 and 90 °C exhibit only one doublet in accordance with one rotameric form. Action of PMe3 on [xxx] (4a) [L - Cl-[CH:]; -P(C6HQ2 (2a)] results in the formation of the cyclic acyl compound [xxx] (5a).

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