- Reaction of TiCl4 with diethyl ether. Experimental and quantum-chemical study
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The reaction of titanium tetrachloride with diethyl ether at various ratios of components and temperatures was studied by the NMR and mass spectrometry methods. The TiCl4·2Et2O complex does not pass in the gas phase. Formation of ethoxytrichlorotitanium among reaction products was established by the X-ray structure analysis. The model of conversion from initial components to titanium dioxide was suggested on the basis of the obtained experimental data and quantum-chemical calculations (B3LYP/def2-SVP level of theory).
- Shugurova,Davydova,Sevast'Yanova,Misharev,Bodensteiner,Scheer
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- SYNTHESIS OF PHOSPHINIMIDE COORDINATION COMPOUNDS
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Methods to make R13P═N—TiCl3 and (1-R2-Indenyl)Ti(N═PR13)Cl2, where R1 is independently selected from C1-30 hydrocarbyl radical which is unsubstituted or further substituted by one or more halogen atom, a C1-8 alkoxy radical, a C6-10 aryl radical, a C6-10 aryloxy radical, an amido radical, a silyl radical, and a germanyl radical; P is phosphorus; N is nitrogen (and bonds to the metal M); R2 is a substituted or unsubstituted alkyl group, a substituted or an unsubstituted aryl group, or a substituted or unsubstituted benzyl group, wherein substituents for the alkyl, aryl or benzyl group are selected from alkyl, aryl, alkoxy, aryloxy, alkylaryl, arylalkyl and halide substituents. The method to make R13P═N—TiCl3 combines a titanium species TiCl3(OR) where R is an alkyl or aromatic group, with a trimethylsilyl phosphinimide compound R13P═N—SiMe3 in the presence of solvent, to give the titanium complex R13P═N—TiCl3. The method to make (1-R2-Indenyl)Ti(N═PR13)Cl2 consists of deprotonating 1-R2-indene with an appropriate base, followed by reaction with R13P═N—TiCl3.
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Paragraph 0113
(2015/02/05)
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