Preparation, Physicochemical Properties, and Crystal Structures of Trifluoroacetic Acid Aminium Salts

IF 0.6 4区 材料科学 Q4 CRYSTALLOGRAPHY
V. V. Semenov, N. V. Zolotareva, N. M. Lazarev, B. I. Petrov, G. K. Fukin, A. V. Cherkasov, T. I. Lopatina, T. I. Kulikova, T. A. Kovylina, E. N. Razov
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引用次数: 0

Abstract

Monoethanolaminium trifluoroacetate (HO‒CH2CH2‒NH\(_{3}^{ + }\) O(O)C‒CF3), triethanolaminium trifluoroacetate ((HO‒CH2CH2)3NH+ O(O)C‒CF3), tris(hydroxymethyl)methanaminium trifluoroacetate ((HO‒CH2)3C-NH\(_{3}^{ + }\) O(O)C‒CF3), and 2,2'-(ethylenedioxy)di(ethylaminium) bis(trifluoroacetate) (CF3-C(O)O‒ +H3N-(CH2CH2O)2CH2CH2-NH\(_{3}^{ + }\) O(O)C‒CF3) were synthesized by the reactions of trifluoroacetic acid with monoethanolamine, triethanolamine, tris(hydroxymethyl)methanamine, and 2,2'-(ethylenedioxy)di(ethylamine), respectively. Ammonium trifluoroacetate (NH\(_{4}^{ + }\) OC(O)CF3) was prepared by the reaction of trifluoroacetic acid with hexamethyldisilazane and with trimethylsilyl trifluoroacetate CF3C(O)OSi(CH3)3. The synthesized compounds are low-melting crystalline salts, which are transferred into a vapor phase upon heating to 200–220°С. The reaction of CF3C(O)OSi(CH3)3 with monoethanolamine afforded monoethanolaminium trifluoroacetate instead of expected 2,2,2-trifluoro-N-(2-hydroxyethyl)acetamide CF3C(O)-NH-CH2CH2OH. The aminium salts were characterized by IR and NMR spectroscopy, mass spectrometry, high-performance liquid chromatography, and scanning electron microscopy. The thermal behavior and thermal stability of the salts were studied by differential scanning calorimetry and thermogravimetry, respectively. The molecular structures of monoethanolaminium trifluoroacetate, triethanolaminium trifluoroacetate, tris(hydroxymethyl)methanaminium trifluoroacetate, and ammonium trifluoroacetate were determined.

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三氟乙酸铵盐的制备、理化性质和晶体结构
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来源期刊
Crystallography Reports
Crystallography Reports 化学-晶体学
CiteScore
1.10
自引率
28.60%
发文量
96
审稿时长
4-8 weeks
期刊介绍: Crystallography Reports is a journal that publishes original articles short communications, and reviews on various aspects of crystallography: diffraction and scattering of X-rays, electrons, and neutrons, determination of crystal structure of inorganic and organic substances, including proteins and other biological substances; UV-VIS and IR spectroscopy; growth, imperfect structure and physical properties of crystals; thin films, liquid crystals, nanomaterials, partially disordered systems, and the methods of studies.
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