Preparation of ceric alkoxides in glycol ethers

Gradeff, Peter S.; Schreiber, Fred G.; Mauermann, Heiko

doi:10.1016/0022-5088(86)90319-x

Cited by 28 publications

(13 citation statements)

References 6 publications

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“…According to Gradeff et al, the reactivity of solvated CAN is crucially influenced by the solvent and base employed , . In reactions of CAN with an alcohol (Scheme , (i) & (ii) ) intricate ammonium‐alkoxide‐nitrate species of cerium are formed under passing of ammonia.…”

Section: Introductionmentioning

confidence: 93%

“…The latter reaction is driven by the precipitation of the side product NaNO 3 . However, in coordinating solvents like DME and THF, NH 4 NO 3 engages in a consecutive reaction with the generated cerium(IV) alkoxides affording unidentified NH 4 NO 3 ate complexes (Scheme , (iv) ) …”

Section: Introductionmentioning

confidence: 99%

“…[8,9h] According to Gradeff et al, the reactivity of solvated CAN is crucially influenced by the solvent and base employed. [10,11] In organoammonium chloride side products, the salt-metathesis route gave good yields for homoleptic [Ce{OSi(OtBu) 3 } 4 ]. The CAC R /alkylsiloxide reaction mixtures also suffer from (photo)redox processes as revealed by the formation of trivalent [Ce(OSiiPr 3 ) 4 (NMe 4 )], but can be further stabilized by pyridine coordination as shown for the solid-state structure of [Ce-(OSiiPr 3 ) 4 (py)].…”

Section: Introductionmentioning

confidence: 99%

“…However, in coordinating solvents like DME and THF, NH 4 NO 3 engages in a consecutive reaction with the generated cerium(IV) alkoxides affording unidentified NH 4 NO 3 ate complexes (Scheme 1, (iv)). [11] A stepwise partial alkoxy-nitrato exchange reaction is feasible as described by Evans et al for bimetallic complex [{Ce(OtBu) 6 Na 2 }(THF) 4 ] (Scheme 1, (v)). [8] Recently, the ceric ammonium chloride (Et 4 N) 2 [CeCl 6 ] (CAC Et ) was found to provide a convenient entry into tetravalent cerium chemistry.…”

Section: Introductionmentioning

confidence: 99%

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Ceric Ammonium Nitrate and Ceric Ammonium Chloride as Precursors for Ceric Siloxides: Ammonia and Ammonium Inclusion

et al. 2018

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Treatment of ceric ammonium nitrate (CAN) with sodium tris(tert‐butoxy)siloxide in THF afforded crystalline complexes [Ce{OSi(OtBu)3}3(NO3)(NH3)2(THF)] and [Ce{OSi(OtBu)3}4(NH3)2] featuring strong ammonia coordination. Conducting the CAN/NaOSi(OtBu)3 (1:4) reaction in acetonitrile gave ceric ate complex [Ce{OSi(OtBu)3}3(NO3)2(NH4)(NCCH3)] where the ammonium cation is embedded in the siloxy ligand sphere via hydrogen bonding. Salt‐metathetic conversion of ceric organo(R)ammonium hexachlorides (CACR, R = Me, Et) with NaOSi(OtBu)3 and sodium siloxides NaOSiR3 (R = Et, iPr) in THF allowed the isolation of ceric siloxide complexes [Ce{OSi(OtBu)3}4], [Ce(OSiEt3)4(THF)0.5], and [Ce(OSiiPr3)4]. Although the reaction products are prone to ate complex formation with the organoammonium chloride side products, the salt‐metathesis route gave good yields for homoleptic [Ce{OSi(OtBu)3}4]. The CACR/alkylsiloxide reaction mixtures also suffer from (photo)redox processes as revealed by the formation of trivalent [Ce(OSiiPr3)4(NMe4)], but can be further stabilized by pyridine coordination as shown for the solid‐state structure of [Ce(OSiiPr3)4(py)]. The siloxide complexes were characterized by NMR, DRIFT, UV/Vis spectroscopy and cyclic voltammetry, as well as paramagnetic susceptibility measurements, X‐ray structure, and elemental analysis. The electrochemical studies revealed an effective stabilization of the CeIV ion within the siloxy ligand environments.

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Section: Introductionmentioning

confidence: 93%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Ceric Ammonium Nitrate and Ceric Ammonium Chloride as Precursors for Ceric Siloxides: Ammonia and Ammonium Inclusion

et al. 2018

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“…Following this step, the ltrate was evaporated to 10 percent its initial volume and used as it was for the ceria synthesis. 19,20 The chemical structure and properties of the concentrate were identied and characterized by ATR-FTIR 19-24 and 1 H & 13 C NMR spectroscopy. 25…”

Section: Preparationmentioning

confidence: 99%

Surface properties of ceria synthesised using Triton-X based reverse microemulsions

Paschalidou

Theocharis

2019

RSC Adv.

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The effect of the tail length of Triton-X surfactants on the surface properties of ceria prepared by means of reversed micelles and Ce(O i Pr) 4 has been systematically studied. Generally, solids with increased surface areas (up to 136 m 2 g À1 ) were synthesised. It was shown that the tail length strongly affects the surface characteristics. Further studies were carried out using UV-Vis, ATR-FTIR, XRD and TGA/DSC studies of the precursor gels as well as N 2 -isothermal adsorption BET, XRD, FT-IR, UV-Vis diffuse reflectance and SEM investigations of the final solids samples. An interaction mechanism between the ceria precursor molecules and the polar tail of the reversed Triton X micelles and the formation of ceria (CeO 2 ) particles in the aqueous nucleus of the reversed microemulsions is proposed.

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Lanthanoiden‐Komplexe, I Solvensfreie Alkoxid‐Komplexe des Neodyms und Dysprosiums. Kristall‐ und Molekülstruktur von trans‐Bis(acetonitril)tris(tri‐tert‐butylmethoxy)neodym

et al. 1992

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Molecular Structure of frans-Bis(acetonftrile)tris(tri-ferf-buty~e~oxy)ne~ymiumThe first lanthanide complex 3a is obtained from the sterically Under the same conditions D Y [ N { S~( C H~)~)~]~ (2b) yields the demanding silanol (tC,H9)3SiOH (silox", la) and Nd-homoleptic ditox derivative 6. The new complexes are all very p{Si(CH3)3)d3 (2a). Similarly, the bulky alcohols hitox-H', soluble in aliphatic hydrocarbons. They show a very different tri-tert-butylmethanol (1 b), and "ditox-H", di-tert-butylme-thermal stability as, for example, expressed in their sublimathan01 (lc), react with 2a to give the corresponding alkoxide tion behaviour.

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Preparation of ceric alkoxides in glycol ethers

Cited by 28 publications

References 6 publications

Ceric Ammonium Nitrate and Ceric Ammonium Chloride as Precursors for Ceric Siloxides: Ammonia and Ammonium Inclusion

Ceric Ammonium Nitrate and Ceric Ammonium Chloride as Precursors for Ceric Siloxides: Ammonia and Ammonium Inclusion

Surface properties of ceria synthesised using Triton-X based reverse microemulsions

Lanthanoiden‐Komplexe, I Solvensfreie Alkoxid‐Komplexe des Neodyms und Dysprosiums. Kristall‐ und Molekülstruktur von trans‐Bis(acetonitril)tris(tri‐tert‐butylmethoxy)neodym

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