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Institute
A convenient and new entry into the chemistry of highvalent pentamethylcyclopentadienyl halfsandwich complexes of molybdenum and tungsten is described. The reaction of Mo-(NtBu)\(_2\)Cl\(_2\) or W(NtBu)\(_2\)Cl\(_2\)(py)\(_2\) with Cp*Li (Cp* = \(\eta^5\)-C\(_5\)Me\(_5\)) provides a high-yield route to new complexes Cp*Mo-(NtBu)\(_2\)CI (la) and Cp*W(NtBu)\(_2\)Cl (1 b) which are converted into a variety of diimido, monoimido, and oxo derivatives. Treatment of 1 a, b with MeLi yields the highly volatile methyl derivatives Cp*Mo(NtBu)\(_2\)Me (2a) and Cp*W(NtBu)\(_2\)Me (2b), while protolysis of 1 a, b with an excess of HCI gas leads to selective cleavage of only one imido function with formation of Cp*Mo(NtBu)Cl\(_3\) (3a) and Cp*W(NtBu)Cl\(_3\) (3b). In contrast, protolysis of 1 a, b with aqueous HCI provides a high-yield route to the well-known organometallic oxides [Cp*MoO\(_2\)](μ-0) (4a) and [Cp*WO\(_2\)](\(\mu\)-0) (4b). These two key compounds are easily converted into the organomolybdate and organotungstate salts NBu\(_4\)[Cp*MoO\(_3\)] (5a) and NBu\(_4\)[Cp*WO\(_3\)] (Sb) by cleavage of the M - 0 - M bridge with NBu\(_4\)[OH]. The Xray structure of 3a is reported.
Chiral 2-alkylbranched acids, esters and alcohols. Preparation and stereospecific flavour evaluation
(1991)
Racemic 2-alkylbranched acids are transformed to diastereomeric derivatives with (S)-2-hydroxy-3-phenylpropionic acid-N-methylamide or (S)-(-)-l-phenylethylamine and separated by liquid chromatography to pure diastereoisomers, which are subsequently hydrolyzed to yield optically pure acids. Enantiomeric alcohols are generated by LiAlH4-reduction of the corresponding acids, esters are synthesized by different methods. The odour impression of the enantiomeric compounds is investigated.
Physical properties of active materials built up from small molecules are dictated by their molecular packing in the solid state. Here we demonstrate for the first time the growth of n-channel single-crystal field-effect transistors and organic thin-film transistors by sublimation of 2,6-dichloro-naphthalene diimide in air. Under these conditions, a new polymorph with two-dimensional brick-wall packing mode (\(\beta\)-phase) is obtained that is distinguished from the previously reported herringbone packing motif obtained from solution (\(\alpha\)-phase). We are able to fabricate single-crystal field-effect transistors with electron mobilities in air of up to 8.6 cm\(^{2}\)V\(^{-1}\)s\(^{-1}\) (\(\alpha\)-phase) and up to 3.5 cm\(^{2}\)V\(^{-1}\)s\(^{-1}\) (\(\beta\)-phase) on n-octadecyltriethoxysilane-modified substrates. On silicon dioxide, thin-film devices based on \(\beta\)-phase can be manufactured in air giving rise to electron mobilities of 0.37 cm\(^{2}\)V\(^{-1}\)s\(^{-1}\). The simple crystal and thin-film growth procedures by sublimation under ambient conditions avoid elaborate substrate modifications and costly vacuum equipment-based fabrication steps.