The Orthogonal (e,e,e)‐Tris‐Adduct of 9,10‐Dimethylanthracene with C60‐Fullerene: A Hidden Cornerstone of Fullerene Chemistry. Preliminary Communication

Tris(9′,10′‐dimethyl[9,10]ethanoanthracene[11′,12′: 1,9;11″,12″: 16,17;11′′′,12′′′: 30,31])[5,6]fullerene C₆₀, the orthogonal (e,e,e)‐tris‐adduct of C₆₀ and 9,10‐dimethylanthracene, was obtained from [4+2]‐cycloaddition (Diels–Alder reaction) at room temperature. The thermally unstable orange red (e,e,e)‐tris‐adduct was purified by chromatography and was isolated in the form of red monoclinic crystals. Its C₃‐symmetric addition pattern was established spectroscopically. Its structure could be further investigated by single crystal X‐ray diffraction. The (e,e,e)‐tris‐adduct of C₆₀ and 9,10‐dimethylanthracene has earlier been suggested as intermediate and reversibly formed critical component in ‘template directed’ addition reactions of C₆₀. This previously elusive compound has now been isolated and structurally characterized.     

Organoalkoxochlorogallane

Organoalkoxochlorogallanes Me₂GaCl was treated with ⁿBuOH and ⁱBuOH in a molar ration of 1:2, respectively. However, only one equivalent of the alcohol reacted with MeGaCl₂ to give [MeGa(Cl)OⁿBu]₃ ( 1 ) or [MeGa(Cl)OⁱBu]₃ ( 2 ). 1 and 2 were characterized by NMR and IR techniques as well as by X‐ray structure determinations. According to that 1 and 2 form trimers in solution and the solid state. In solution both isomers C_s and C_3v were observed while the trimers exist only as C_s isomers in the solid state which exhibit strongly distorted boat conformations with a disorder of the Cl/Me position at one of the gallium atoms.     

Convenient multigram synthesis of monodisperse oligo(ethylene glycols): effective reaction monitoring by infrared spectroscopy using an attenuated total reflection fibre optic probe

A convenient approach for the synthesis of monodisperse oligo(ethylene glycols) up to 12 units is described. A novel cleavage protocol replacing laborious hydrogenolysis is introduced to achieve a fast, inexpensive and widely applicable procedure. In addition to the synthetic part, Fourier transform infrared (FTIR) spectroscopy using a fibre optic attenuated total reflection (ATR) sensor was applied to monitor the formation of sensitive key intermediates, resulting in optimized reaction times. By applying this in-line technique, the possibility of real-time analysis under inert conditions was impressively demonstrated.     

An NMR investigation on the phase structure and molecular mobility of the novel exfoliated polyethylene/palygorskite nanocomposites

Novel exfoliated polyethylene (PE)/palygorskite nanocomposites prepared by in situ polymerization are characterized by solid‐state nuclear magnetic resonance (NMR). The phase structure and molecular mobility are investigated by a combination of proton and carbon NMR. The results showed that incorporation of small amounts of palygorskite had great influence on the phase structure and molecular mobility. The incorporated palygorskite hindered the crystallization process and introduced motion‐hindered chains in the NMR crystalline and amorphous phase. ¹³C cross‐polarization and magic‐angle spinning NMR revealed two orthorhombic crystalline phase with different line‐width. The chain mobility of orthorhombic crystalline phase with broad resonance line is obviously hindered compared with the phase with narrow resonance line when the filler is introduced. Additionally, the results of pulsed field gradient NMR technique show those the tortuosities in the nanocomposites are much higher than that in the bulk PE. The self‐diffusion process of probe molecules is also influenced by the palygorksite load. © 2010 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 1363–1371, 2010