Reactions of (CF3)3BCO with Amines and Phosphines

Finze, Maik; Bernhardt, Eduard; Willner, Helge; Lehmann, Christian W.

doi:10.1021/ic0515305

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Reactions of (CF₃)₃BCO with Amines and Phosphines

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Lehmann, Christian W.
Service Department Lehmann (EMR), Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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引用

Finze, M., Bernhardt, E., Willner, H., & Lehmann, C. W. (2006). Reactions of (CF₃)₃BCO with Amines and Phosphines. Inorganic Chemistry, 45(2), 669-678. doi:10.1021/ic0515305.

引用: https://hdl.handle.net/11858/00-001M-0000-000F-944D-8

要旨

Reactions of tris(trifluoromethyl)borane carbonyl, (CF₃)₃BCO, with ammonia yielded either a mixture of [NH₄][(CF₃)₃BC(O)NH₂], [NH₄][(CF₃)₃BCN], and [NH₄]₂[{(CF₃)₃BC(O)}₂NH] or neat [NH₄]₂[{(CF)BC(O)}NH] depending on the reaction conditions. The salt K[(CF₃)₃BC(O)NH] was obtained as the sole product from the reaction of NH₃ with K[(CF₃)BC(O)F]. A simple synthesis for cyanotris(trifluoromethyl)borates, M[(CF)₃BCN], was developed by dehydration of M[(CF)₃BC(O)NH] (M = [NH₄], K) using phosgene. In addition, syntheses of the tris(trifluoromethyl)boron species [(CF₃)BC(O)NHⁿPr]^-, [(CF₃)₃BC(O)NMe]^-, and (CF₃)BC(O)NMe₃, as well as of (CF)BC(O)PMe, were performed. All species were characterized by multinuclear NMR spectroscopy. As far as neat substances resulted, IR and Raman spectra were recorded and their thermal behaviors were studied by differential scanning calorimetry. The interpretation of reaction pathways, structures, and vibrational spectra are supported by DFT calculations. The solid-state structure of K₂[{(CF₃)BC(O)}NH]·2MeCN was determined by single-crystal X-ray diffraction.