Ana Sofia Diogo FerreiraUniversidade NOVA de Lisboa | NOVA · UCIBIO
Ana Sofia Diogo Ferreira
PhD Chemistry
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28
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Introduction
Liquid and semi-solid NMR techniques applied towards unravelling unconventional solvents interactions and dynamics.
Publications
Publications (28)
Cucurbiturils are popular macrocyclic receptors that bind complementary guest molecules with high affinity in aqueous environments. They are recognized for their ability to selectively bind positively charged guest molecules, including ionizable ammonium cations which frequently display much higher affinity than their neutral counterparts. This sel...
Proteins have wide biological activities facilitating their employment in several applications from academia to industry. Their implementation depends on costly downstream processes yielding proteins with high purity, stability, and activity. Ionic liquids (ILs) have emerged in the field of protein extraction and purification as an asset due to the...
The conformational changes of the homooxa adamantyl ketones 1 and 2, as well as of the calix[4]arene analogue derivative 3, all in the cone conformation, upon Pb²⁺ complexation were investigated by ¹H, ¹³C, ²⁰⁷Pb NMR and proton spin-lattice relaxation times (T1) experiments. The X-ray crystal structures of ketones 1 and 3 were determined. The inclu...
Deep Eutectic Systems (DESs) are an emerging class of green solvents with a myriad of applications, from biotechnology to material science. The high viscosity of most DESs is an obstacle that can be circumvented by the addition of water. But how much water is too much water? There is a need to understand the effect of water in the organizational dy...
Fucus spiralis that was collected in the four seasons was submitted to an extraction with ethanol:water (crude extracts Et80), followed by a liquid–liquid fractionation with organic solvents (fraction He from n-hexane; aqueous fractions AQ1, AQ2, AQ3 and AQ4; ethyl acetate fraction EA), with the aim of obtaining phlorotannin-enriched extracts. All...
The selective photodeprotection of the NVoc-modified FGG tripeptide yields the transformation of its 1:1 receptor-ligand complex with cucurbit[8]uril into a homoternary FGG2@CB8 assembly. The resulting light-induced dimerization of the model peptide provides a tool for the implementation of stimuli-responsive supramolecular chemistry in biologicall...
In the last few years, ionic liquids (ILs) have been the focus of extensive studies concerning the relationship between structure and properties and how this impacts their application. Despite a large number of studies, several topics remain controversial or not fully answered, such as: the existence of ion pairs, the concept of free volume and the...
Ionic liquids have been on the spotlight of chemical research field in the last decades. Their physical properties (low vapor pressure, thermal stability, and conductivity) and the possibility of fine tuning make them a versatile class of compounds for a wide range of applications, such as catalysis, energy, and material sciences. Ionic liquids can...
The imidazolium-based ionic liquids (ILs) are solvents known for selectively solubilizing CO 2 from a gas CH 4 /CO 2 mixture, hence we have produced new hybrid adsorbents by immobilizing two ILs on xerogel silica to obtain a solid-gas system that benefits the ILs' properties and can be industrially applied in CO 2 capture. In this work, the ILs (Me...
The imidazolium-based ionic liquids (ILs) are solvents known for selectively solubilizing CO2 from a gas CH4/CO2 mixture, hence we have produced new hybrid adsorbents by immobilizing two ILs on xerogel silica to obtain a solid–gas system that benefits the ILs’ properties and can be industrially applied in CO2 capture. In this work, the ILs (MeO)3Si...
In this work, [Bmim][BF4]/water mixtures were analysed over the whole water composition (xw) in order to study the rotational and translational behaviour of the ions. We employed a multinuclear NMR approach to determine anion/cation/water diffusion coefficients and longitudinal relaxation rates at different water content. In neat IL the cation diff...
THEDES, so called therapeutic deep eutectic solvents are here defined as a mixture of two components, which at a particular molar composition become liquid at room temperature and in which one of them is an active pharmaceutical ingredient (API). In this work, THEDES based on menthol complexed with three different APIs, ibuprofen (ibu), BA (BA) and...
We applied Pulsed Gradient Spin Echo diffusion with high-resolution magic angle spinning NMR to study sol-gel matrices used to encapsulate enzymes for biocatalysis (TMOS/MTMS and TMOS/BTMS) to gain insight into the local chemical microenvironment. Transport properties of solvents with different polarities (1-pentanol, acetonitrile and n-hexane) wer...
New acyl hydrazones were synthesized by condensation with camphorquinone aiming at extending the range of applications of the biologically active camphor compounds and structural studies by XRD, 1H-NMR and IR were used in conjunction with advanced computational methodologies to understand the new structural chemistry enabled by the conjugation of t...
A therapeutic deep eutectic system (THEDES) is here defined as a deep eutectic solvent (DES) having an active pharmaceutical ingredient (API) as one of the components. In this work, THEDESs are proposed as enhanced transporters and delivery vehicles for bioactive molecules. THEDESs based on choline chloride (ChCl) or menthol conjugated with three d...
Pulsed field gradient spin echo high resolution magic angle spinning nuclear magnetic resonance spectroscopy is a powerful technique to characterize confined biosystems. We used this approach to assess the diffusion of solvent and reaction species within sol-gel matrices differing in enzyme loading.
The reactivity of 3-oxo-camphorsulfonylimine (1) was explored toward the formation of new organic species in processes strictly organic or catalyzed by platinum. Synthesis and characterization of (1S)-1-[7,7-dimethyl-2-(4-ethinylphenylimino)-3-oxo-bicyclo[2.2.1]heptanyl]-methanesulfonamide (2), (3aS,7R)-7-hydroxy-8,8-dimethyl-7-(N-methylamino-1-pro...
Seven new camphor palladium or platinum compounds with novel metal coordination environments were obtained by convenient choice of the experimental conditions in particular the solvent. cis-[PtCl2(PhNC10H14O)2]) and [Pd(MeNNC10H14O)2] were structurally characterized by X-ray diffraction analysis while [{PtCl2(Me2NC10H13NSO2)}2], [{PdCl2(YNC10H14O)}...
The cooperative effect of the camphor imine ligand (YNC10H14O) in the cyclization of 5-hexyn-1-ol and 4-pentyn-1-ol promoted by complexes trans-[MCl2(YNC10H14O)2] (M=Pd, Y=NH2, NHMe, NMe2, OH, Ph; Pt, Y=NH2, NHMe, NMe2) is established from a direct relation between the constants calculated for conversion of 5-hexyn-1-ol (A) into 2-methyl-2-pent-4-y...
Conversion of 4-pentyn-1-ol (A) into 2-methyl-2-pent-4-ynyloxy-tetrahydrofuran (B) is catalysed by camphorimine complexes trans-[PdCl2(YNC10H14O)2] (Y=NMe2, NHMe, NH2, OH, OMe, Pri, Ph), trans-[PdBr2(YNC10H14O)2] (Y=NMe2, NH2, OH, Ph), trans-[PtCl2(YNC10H14O)2] (Y=NMe2, NHMe, NH2). In the presence of H2O those catalysts further promote the conversi...
Synthesis and characterization of camphor-derived ligands and novel Ni-based complexes.
Copper(I) chloride was found to be a highly efficient reagent to promote the cleavage of acetylenic sub-stituents from the camphor skeleton of compounds 1 containing two C–C triple bonds as well as from the compounds 6 and 7 containing one. This is a formal reversal of the formation of these compounds by the reaction of acetylides with keto and imi...
The properties of [NiX(PR2CH2C(But)NNC(But)CH2PR2)]+ complexes (where X = Br, and R = cyclohexyl (Cy), isopropyl (Pri), tert-butyl (But), phenyl (Ph); X = Cl or I, and R = cyclohexyl) as catalysts for the polymerisation of ethylene were evaluated with or without the co-catalysts methylaluminoxane (MAO), diethylaluminium chloride, trimethylaluminium...
3-Hydrazonocamphor, 3-(RR<sup>1</sup>NN)C<sub>10</sub>H<sub>14</sub>O (R = Me, R<sup>1</sup> = H), undergoes intramolecular hydrogen bridging by coordination to platinum or palladium. This effect is evidenced by considerable decrease in the ν(C=O) frequency (compared to the free ligand) in the IR spectra of the complexes [MCl<sub>2</sub>L<sub>2</su...
The cyclization of 3- or 4-pentyn-1-ol is catalysed by PdCl2 or trans-[PdCl2L2] (L=R-camphorimine; R=Ph; Pri; NMe2) complexes at room temperature affording heterocyclic compounds, respectively, 2-methyl-2-pent-3-ynyloxy-tetrahydrofuran or 2-methyl-2-pent-4-ynyloxy-tetrahydrofuran which subsequently add water to give selectively 5-(2-methyl-tetrahyd...
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How to grow ammonium dihydrogen phosphate crystals by heterogeneous nucleation "On the Rocks", in solutions with food dyes. Occlusion of dyes in the crystal Lattice of ADP
Questions
Questions (2)
I am seeing to buy a glove box system (not to big) to handle moist sensitive samples. Can anybody suggest me based on their experience? Oxygen is not, for now, a concern, just moisture since most my samples are hygroscopic. As always money is a problem so I need to balance money/performance very carefully.
Thanks in advance.
When I was trying to prepare ILs using lactic acid I found that independently of brand or purity there is also contamination of low molecular weight polymers. I've tried fractional distillation (as described in Armarego book) but it did not solve. Does anyone have a suggestion to obtain high purity lactic acid?thanks in advance