Trifluoroacetamide CF3C(O)NH2, N,N'-bis(trifluoroacetyl)ethylenediamine CF3C(O)NHCH2CH2HN(O)CCF3, trifluoroacetyl-2-aminoethanol CF3C(O)NHCH2CH2ОН, and 1,2-bis(trifluoroacetylaminoethoxy)ethane CF3C(O)NHCH2CH2ОCH2CH2ОCH2CH2НN(O)CCF3 were synthesized by the thermal decomposition (200–250°С, Ar) of the corresponding ammonium and aminium salts, such as ammonium trifluoroacetate CF3C(O)O‒ +NH4, N,N'-ethylenediamine bis(trifluoroacetate) CF3COO‒ +NH3CH2CH2H3N+ ‒OOCCF3, 2-aminoethanol trifluoroacetate CF3COO‒ +NH3CH2CH2ОН, and 1,2-bis(aminoethoxy)ethane bis(2-trifluoroacetate) CF3COO‒ +NH3CH2CH2ОCH2CH2ОCH2CH2Н3N+ ‒OOCCF3. The synthesized compounds were characterized by elemental analysis, powder X-ay diffraction, IR and NMR spectroscopy, mass spectrometry, thermogravimetry, optical and scanning electron microscopy. The molecular structure of ethylenediamine N,N'-bis(trifluoroacetate) was determined.
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.
The reaction of hexamethylenetetramine (CH2)6N4 with sparingly soluble (1-hydroxyethylidene)diphosphonates M(H2L)•2H2O (M = Mn, Co, Zn; H4L is (1-hydroxyethylidene)diphosphonic acid) afforded water-soluble compounds of the composition [(CH2)6N4H2]ML•2H2O (M = Mn (1), Co (2), Zn (3)). Manganese derivative 1 lost its solubility during storage, whereas the cobalt and zinc compounds retained it. The tetrafunctional base hexamethylenetetramine reacts with tetrafunctional (1-hydroxyethylidene)-diphosphonic acid H4L in methanol to form hexamethylenetetraminium (1-hydroxyethylidene)diphosphonate dihydrate [(CH2)6N4H]+(H3L)•2H2O (4). When heated in an aqueous methanol medium, compound 4 dissociates to acid H4L and base (CH2)6N4, hexamethylenetetramine reacts with water to produce ammonia and formaldehyde, and the acid H4L and ammonia generate diammonium (1-hydroxyethylidene)diphosphonate (NH4)2H2L. The heating in an inert atmosphere causes the extensive decomposition of compound 4 giving a non-volatile water-soluble residue and a series of volatile organic compounds, such as amines, amides, amino alcohols, and amino acids. The obtained compounds were studied by IR spectroscopy, elemental analysis, powder X-ray diffraction, and thermogravimetric analysis. The molecular structure of diammonium (1-hydroxyethylidene)diphosphonate (NH4)2H2L was determined.
Triethylenediaminium ethylenediaminetetraacetatozincate trihydrate ([HN(CH2CH2)3NH]ZnL⋅ 3H2О) and tetramethylethylenediaminium ethylenediaminetetraacetatozincate dihydrate ([H(CH3)2NCH2CH2N(CH3)2H]ZnL⋅2H2О) were synthesized by the reaction of zinc oxides with ethylenediaminetetraacetic acid and then with its triethylenediaminum or tetramethylethylenediaminium salts. The synthesized compounds were isolated from aqueous solutions or organic solvents as fiber-like, cubic, and pyramidal crystals, which were characterized by elemental analysis, scanning electron microscopy, IR spectroscopy, thermogravimetry, and differential scanning calorimetry.
Zinc(II) bis(3-aminiumpropylsilsesquioxane)(1-hydroxyethylidene)diphosphonate tetrahydrate and manganese(II) bis(3-aminiumpropylsilsesquioxane)(1-hydroxyethylidene)diphosphonate trihydrate were obtained by the reactions of aqueous solution of 3-aminopropyltriethoxysilane with (1-hydroxyethylidene)diphosphonates of zinc(II) H2ZnL·2H2O and manganese(II) H2MnL·3H2O. The synthesized compounds were studied by the methods of elemental, thermal, and X-ray phase analysis, IR spectroscopy, and scanning electron microscopy. The specific surface areas of the initial xerogels and products of their thermal decomposition were measured.
Poorly soluble zinc ethylenediaminetetraacetate zincate Zn[ZnL] reacts with sodium Na 4 L, potassium K 4 L, ammonium (NH 4 ) 4 L, 2-ammonioethanol (H 3 NCH 2 CH 2 OH) 4 L, and hexamethylene-1,6-diammonium {H 3 N(CH 2 ) 6 NH 3 } 2 L salts of ethylenediaminetetraacetic acid H 4 L to give readily soluble sodium Na 2 [ZnL], potassium K 2 [ZnL], ammonium (NH 4 ) 2 [ZnL], 2-ammonioethanol (H 3 NCH 2 CH 2 OH) 2 [ZnL], and hexamethylene-1,6-diammonium {H 3 N(CH 2 ) 6 NH 3 }[ZnL] ethylenediaminetetraacetate zincates. The reaction of tetrakis(triethylammonium) salt {(C 2 H 5 ) 3 NH} 4 L with Zn[ZnL] does not give the expected bis(triethylammonium) ethylenediaminetetraacetate zincate {(C 2 H 5 ) 3 NH} 2 [ZnL], but gives instead mono(triethylammonium) ethylenediaminetetraacetate zincate, {(C 2 H 5 ) 3 NH}H[ZnL]; in aqueous solution, this product generates poorly soluble zinc ethylenediaminetetraacetate H 2 [ZnL(H 2 O)]·2H 2 O, which was studied by X-ray diffraction (CCDC no. 2172274).
New initiator monomers, derivatives of 3,5-di- tert -butyl- o -benzoquinone containing the 2‑hydroxyethyl methacrylate (HEMA) and pentaerythritol triacrylate (PETA) moieties, have been synthesized. The activity of new o -quinones has been examined in the visible light-induced polymerization (coinitiator N , N -dimethylcyclohexylamine) of oligocarbonate dimethacrylate OCM‑2. The thermal stability of the obtained polymers has been studied. Polymers have been prepared by copolymerization of the synthesized o -quinones with HEMA and PETA (initiator azobisisobutyronitrile, 80°C), and the migration of o -quinones from the products has been evaluated.
The effect of the hexadecyltrimethylammonium bromide concentration in the silica sol, which is used to obtain antireflection coatings over silicate glass, on the light transmission of coated glass and the hardness of the coatings was studied. An increase in the concentration of hexadecyltrimethylammonium bromide in the sol from 1.37 × 10 –2 to 5.20 × 10 –2 M increases the maximum light transmission of glass with an antireflective coating from 94.7 to 99.0%, and minimum, from 84.7 to 93.6%, reduces the refractive index of the coating from 1.43 up to 1.27. The 3H–4H coating hardness acceptable for practice can be achieved provided that the maximum light transmission of glass with a single-layer double-sided coating is ≤96.0–97.0%, the refractive index of the antireflection coating is ≥1.35–1.36, and the maximum volume content of nanopores in the coating is not more than 20.0–23.0 vol % .
Some new β-lactams bearing biologically important morpholine ring have been synthesized by acylation of amino β-lactams in the presence of morpholine-4-carbonyl chloride. These novel β-lactams were prepared under mild reaction conditions without any solvent in short reaction times. Their biological activities have been examined against microbial agents such as Staphylococcus aureus (S. aureus), Escherichia coli (E. coli), Pseudomonas aeruginosa (P. aeruginosa) and fungi such as Candida albicans (C. albicans) and Candida glabrata (C. glabrata). They have been also tested against Plasmodium falciparum K14 resistant strain and showed moderate to good IC 50 values.
The thermal decomposition of cluster Nd3I5(S2)(S2N2)(THF)10 (I) at 50–400°C affords a mixture of products among which tetrahydrofuran (THF), sulfur, diiodine, HI, H2S, CS2, S3N6, S3N5, MeI, thiophene, tetrahydrothiophene, diiodobutane, iodobutene, and NdI3 are identified. The treatment of Ln3I5(S2)(S2N2)(THF)10 (Ln = Nd (I), Dy (II)) with phenanthroline (Phen) in THF at room temperature results in the partial substitution of ТНF to form new complexes Ln3I5(S2)(S2N2)(THF)4(Phen)3. The dissolution of compound I in pyridine gives a pyridine (Py) complex Ln3I5(S2)(S2N2)(THF)3(Py)7. The dissolution of compounds I and II in acetonitrile at 20°C is accompanied by the fast rearrangement and fragmentation of the complexes to form LnI3(MeCN)6, [LnI(S2)(MeCN)], and [LnI(S2N2)(MeCN)]. Complex I in THF does not react with white phosphorus, carbon monoxide, fullerene C60, and chromium hexacarbonyl.
Fe-containing nanoparticles have been grown for the first time on the surface of multiwalled carbon nanotubes by metalorganic chemical vapor deposition using iron acetylacetonate, Fe(acac)(3), as a precursor. The resultant hybrid nanomaterial has been characterized by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, and thermogravimetric analysis. The results demonstrate that the synthesized material consists of multiwalled carbon nanotubes whose surface is decorated with iron nanoparticles.
Hydrolysis of tetraethoxysilane in the presence of Pluronic® F127 block-copolymer in a water-alcohol mixture was used to obtain sol-formulations from which antireflection coatings were deposited onto silicate glass by the dip-coating method and then calcined at high temperatures (200–500°C). Electron spectroscopy was used to study the dependence of the optical transmission of glass samples with a coating on the concentration of Pluronic® F127 in the starting sol, introduction of organic additives (toluene) into the sol, and calcination temperature of the glasses obtained. The refractive index and hardness of the film coatings were determined and their surface structure was assessed.
The addition of 0.1—0.5 mol.% of alumina sol causes the increase in hardness of single-layer optical coatings, produced on silicate glass from silica sol at gel setting temperatures of 60—80 °C, from F—H to 7H—9H. Small concentrations of the additive do not affect the light transmission of the coated glasses. Atomic force microscopy has shown the coating surface to be homogeneous, the surface roughness not exceeding 4.0 nm.
It is shown that the hardness of transparent film coatings produced on silicate glass from silicon dioxide sols that contain minor amounts of products formed in hydrolysis of (BuO)4Ti and (BuO)4Zr and are cured at low temperatures of 20–80°C can be raised.
New water-soluble heteroligand complexes of 2-methyl-4-oxo-4 H -pyran-3-olatoneodymium(III) with aliphatic amino acids (glycine, N -methylglycine, and alanine) have been prepared. Within the biological “transparency window” (700–900 nm) of their electronic absorption spectra, narrow bands of Nd 3+ are found: 4 F 7/2 ← 4 I 9/2 ; 4 F 5/2 ← 4 I 9/2 ; 4 F 3/2 ← 4 I 9/2 (750, 810, and 880 nm). Such complexes can be used as markers for biological tissues visualization.
Thin transparent nanoporous silicon dioxide films with low refractive index (1.26–1.30) were formed on a glass substrate by deposition of a formulation that is based on silicon dioxide sol with addition of poly(propylene glycols) at a low gel annealing temperature of 200°C. The maximum optical transmission of glass with these antireflection coatings is 97.5–98.7%.
Charge transfer complexes of a series of -substituted dimethylanilines with C fullerenes were studied by electron absorption spectroscopy. Energies of charge transfer bonds depend on three effects of substituents in the donor molecule (the inductive, resonance, and polarization effects) with domineering of the resonance effect. The energies are linearly proportional to the potentials of electrochemical oxidation of aniline derivatives.