- Process for the preparation of bistriphenylsilyl chromate
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Disclosed is a process for the preparation of bistriphenylsilyl chromate, wherein triphenylchlorosilane, potassium dichromate and any one selected from alkali metal oxides, alkali hydroxides and alkali metal carbonates are reacted in, as solvent, a mixture of glacial acetic acid and a hydrocarbon solvent at a certain temperature, whereby bistriphenylsilyl chromate having high purity can be obtained with high yield.
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- Chromyl complexes with aryloxy and siloxy ligands
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Interaction of CrO3 and 1 equiv of Ph3CCl in dichloromethane yields a mixture of CrO2Cl2, CrO2Cl(OCPh3) (1), and CrO2-(OCPh3)2 (2). Fractional crystallization gives pure samples of red 1 and orange 2, which have been characterized by X-ray diffraction. Crystal data for 1: space group P1; a = 9.913 (3), b = 10.173 (3), c = 9.019 (3) ?; α = 92.93 (2), β = 92.74 (2), γ = 110.84 (3)°; Z = 2; R1 = 0.044, R2 = 0.059. Crystal data for 2: space group C2/c; a = 23.857 (6), b = 8.759 (3), c = 15.105 (5) ?; β = 110.48 (3)°; Z = 4; R1 = 0.036, R2 = 0.057. A similar result was obtained on reaction of CrO3 and 1 equiv of Ph3SiCl, giving CrO2Cl2, CrO2Cl(OSiPh3) (3), and CrO2(OSiPh3)2 (4). These results are compared with the in situ systems CrO3/Me3SiCl and CrO3/Me3SiOSiMe3, which have been studied by 1H NMR spectroscopy and EI mass spectrometry.
- Stavropoulos, Pericles,Bryson, Nathan,Youinou, Marie-Thérèse,Osborn, John A.
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p. 1807 - 1811
(2008/10/08)
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