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Updated: Feb 22, 2026

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives
Published on: January 19, 2016
[TcII(NO)(trifluoroacetate)4F]2- - synthesis and reactions
S M Balasekaran1, A Hagenbach, M Drees
1Freie Universität Berlin, Institute of Chemistry and Biochemistry, Fabeckstr. 34/36, 14195 Berlin, Germany. ulrich.abram@fu-berlin.de.
Abstract:
Fluoridotetrakis(trifluoroacetato)nitrosyltechnetate(ii) was prepared by the dissolution of Cs2[Tc(NO)F5] in trifluoroacetic acid and addition of (NBu4)F·3H2O. The compound crystallizes as a mixed Cs+/NBu4+ salt in the form of green crystals. Unlike the [Tc(NO)F5]2- salts, the product is soluble in organic solvents and can be used as a precursor for ongoing ligand exchange procedures with organic ligands. The corresponding reactions with triphenylphosphine (PPh3), 1,2-bis(diphenylphosphino)ethane (DPPE) or pyridyldiphenylphosphine (pyPPh2) give technetium(i) complexes of the compositions Cs[Tc(NO)(PPh3)2(CF3COO)2F], [Tc(NO)(DPPE)2(OOCCF3)](PF6) and [Tc(NO)(κN,P-pyPPh2)(κP-pyPPh2)(CF3COO)2]. The products were studied spectroscopically and by X-ray diffraction. The 99Tc NMR resonances of the novel Tc(i) nitrosyls appear between -627 and +952 ppm, which is at a remarkably high field and in the range where normally the signals of Tc(iii) compounds are observed.
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