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Carbonyl olefination with a lithiomethane, having besides the group P(O)Ph2 at the methane C-atom an organo-heavy-metal group, occurs at low temperatures to give exclusively diphenylphosphoryl substituted olefins.  相似文献   

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Ohne Zusammenfassung
Evaluation in HPLC using photodiode-array detectors
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Two New Alkylimido-Methylgallanes with Cage Structure The tetrameric alkylimido-methylgallanes (MeGa? NR)4 (R = CH(CH3)2 ( iPr), C(CH3)3 ( tBu) and Me = CH3) have been prepared by pyrolyses of the dimeric amido compounds (Me2Ga? N(H)R)2 at 250–260°C. The mass, NMR and vibrational spectra are discussed, they prove almost identical structures of the skeletons. The X-Ray structure determination of (MeGa? NtBu)4 shows four heterocubane molecules in the trigonal unit cell (space group P3 c1, a = b = 1061.7(1), c = 3191.8(5) pm) and two disordered benzene solvate molecules. The Ga? N bonds range between 198.4 to 199.9 pm, the Ga? N? Ga and N? Ga? N bond angles lie between 90.6 to 91.4 and 88.6 to 89.2°, respectively. The structure was refined to an R1(R2)-value of 0.049 (0.057).  相似文献   

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Mono(1,3-diene)tris(PR3)iron(0) complexes and bis(1,3-diene)mono(PR3)iron(0) complexes can be synthesized by reduction of FeCl2 with magnesacyclopent-3-ene or activated Mg in the presence of 1,3-dienes and the appropriate PR3 (R = Me, Et, Prn, Cy) ligand. How the various substituted bis(1,3-diene)PR3Fe0 complexes can be obtained from the thermally unstable 1,3-butadiene-tris(PR3)Fe0 complexes by addition of 1,3- or 1,5-dienes is shown. The NMR spectra of these complexes indicate that they are square-pyramidal. This geometry was confirmed by a crystal structure analysis of 1,5-COD-1,3-butadiene-iron(0)-PEt3. The probable mechanism of formation of these novel iron(0) complexes is discussed and their characteristic properties are described.  相似文献   

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Analytical and Bioanalytical Chemistry - Die Versuche wurden unter verständnisvoller Mitarbeit von Frl. C. Mäkelt durchgeführt.  相似文献   

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