Reactions retrodieniques—IX

Ripoll, Jean‐Louis; Lebrun, H.; Thuillier, André

doi:10.1016/0040-4020(80)80229-8

Cited by 42 publications

(18 citation statements)

References 32 publications

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“…0.0868 (5) N32 0.1819 (5) (4) 0.2301 (5) 0.1755 (5) 0.1461 (4) 0.3921 (4) 0.4033 (4) 0.3349 (4) 0.2811 (5) 0.2126 ( I ) 0.049 0.0897 (1) 0.052 0.1722 (3) 0.049 0.0193 (3) 0.040 -0.0028 (3) 0.039 0.1077 (4) 0.042 -0.0464 (4) 0.040 -0,0593 (4) 0.042 0.0326 (4) 0.042 0.2662 (5) 0.045 0.2906 (6) 0.067 0.3371 (7) 0.089 0.3592 (6) 0.084 0.3373 (6) 0.076 0.2908 (5) 0.067 -0.0936 (5) 0.050 -0.0589 (5) 0.053 0.0108 ( 5 ) 0.045 -0.1220 (5) 0.056 -0.1044 (5) 0.063 -0.0300 (5) 0.051 0.0481 (6) 0.055 0.1339 (5) 0.059 0.1694 (5) 0.052 -0.0519 (5) 0.052 (4) 0.4870 (6) 0.4717 (7) 0.03904 (2) 0.1422 (1) 0.0802 (2) -0.0606 (3) 0.1536 (4) -0.0207 (4) 0.0200 (4) (4) z l c 0.01802 (2) -0.0611 (2) 0.0536 (2) 0.1359 (5) 0.1243 (5) 0.0206 (5) -0.0790 (6) -0.0196 (7) 0.29404 …”

Section: Methodsunclassified

Multiple bonds between main-group elements and transition metals. 91. High-oxidation-state rhenium complexes containing the hydridotris(1-pyrazolyl)borato ligand

Degnan¹,

Behm²,

Cook³

et al. 1991

Inorg. Chem.

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2165Bulk Susceptibility Mmurements. The raw data (XRT = 3.58x 10-4 emu/mol) were corrected for temperature-independent diamagnetism (xd = -4.90 X lo4 emu/mo1)22 to afford the paramagnetic susceptibility xiT = 8.54 X lo-' emu/mol. This value is significantly larger than that of [Ni(tmp)12[Re04] (xi, Pt-spine conductors. The rhenium(VI1) complex [ H B ( p~)~l R e 0~ (1) is readily reduced by triphenylphosphine in the presence of excess (CH,)$iX (X = Br, Cl) to give the corresponding rhenium(V) complexes [HB(pz),]ReOX, (2, X = CI; 3, X = Br, pz = pyrazolyl (ClH1N2)).[HB(pz),]ReOCI2 (2), which seems to exist as two bond stretch isomers, reacts with 1 equiv of thiophenol in refluxing THF In the presence of a base [DBU or N(C,H,)J to give [HB(pz),]ReO(CI)(SC,H,) (4). Two equivalents of thiophenol reacts with 2 in refluxing THF, also in the presence of base, to give [ H B (~Z ) , ] R~O ( S C~H~)~ (5). 2 will react with 1.2-ethanedithiol or 1,2-benzenedithiol under similar conditions to give [HB(pz)l]ReO(S2C,H4) (6) and [HB(pz),]ReO(S2C2H4) (7), respectively. The solid-state structures of 4 and 5 have been determined by X-ray crystallography. Both were found to be monomeric with an approximately octahedral arrangement of ligands around the rhenium atoms. 4 crystallizes in the orthorhombic space group Pbcu (No. 61) with cell parameters a = 13.159 ( I ) A, b = 18.656 ( I ) A, c = 15.902 ( I ) A, V = 3904 ( I ) AI, Z = 8, R = 0.043, and R, = 0.031 for 271 3 reflections with I > 244). 5 crystallizes in the monoclinic space group P2Jc (No. 14) with cell parameters a = 15.594 (3) A, b = 21.624 (1) A, c = 15.931 (1) A, @ = 107.00 (I)', V = 5137 (1) AI, Z = 4, R = 0.050, and R, = 0.036 for 6683 reflections with I > 2 4 .

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Section: Methodsunclassified

Multiple bonds between main-group elements and transition metals. 91. High-oxidation-state rhenium complexes containing the hydridotris(1-pyrazolyl)borato ligand

Degnan¹,

Behm²,

Cook³

et al. 1991

Inorg. Chem.

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“…This observation, which finds scarce literature precedent, a,b allowed isolation of vinyl bis (silylamines) as stable molecules. The parent vinylamines are usually unstable and decompose gradually even at low temperatures . The use of this method permitted also facile D‐labelling of the amine resulting from the double deuterosilylation of cinnamonitrile (Figure and entry 8 of Table ).…”

Section: Resultsmentioning

confidence: 99%

Large‐scale preparation and labelling reactions of deuterated silanes

Campos

Rubio

Esqueda

et al. 2011

Labelled Comp Radiopharmac

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A catalytic synthesis of deuterated silanes SiEt 3 D, SiMe 2 PhD and SiPh 2 D 2 is reported that allows their facile generation in a 3-4 g scale, utilizing D 2 (0.5 bar) as the hydrogen isotope source and low catalyst loadings (0.01 mol%). The catalyst precursor is the rhodium (III) complex 1, which contains a (h 5 -C 5 Me 5 )Rh cation stabilized by coordination to a cyclometallated phoshine PMeXyl 2 (Xyl = 2,6-C 6 H 3 Me 2 ). The same complex is also an active catalyst for the hydrosilylation of the C= =O and CN bonds of various ketones, aldehydes and a,b-unsaturated nitriles. Hence, combination of these two properties permits development of a simple and proficient one-flask, two-step procedure for the deuterosilylation of these substrates.

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“…Unlike the other structural isomers of C 2 H 5 N, N-methylenemethylamine (33,34), ethylideneimine (35), and vinylamine [593- (36,37) and the analogous phosphorus compound, phosphirane (38), ethyleneimine is stable at room temperature provided CO 2 is excluded from the air (39). Unexpectedly, ethyleneimine has the highest calculated relative heat of formation of the C 2 H 5 N isomers (40).…”

Section: Chemical Propertiesmentioning

confidence: 99%