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The Pd-catalyzed annulative π-extension of 1,8-dibromonaphthalene for the preparation of fluoranthenes in a single operation has been investigated. With specific arenes such as fluorobenzenes, the Pd-catalyzed double functionalization of C–H bonds yields the desired fluoranthenes. The reaction proceeds via a palladium-catalyzed direct intermolecular arylation, followed by a direct intramolecular arylation step. As the C–H bond activation of several benzene derivatives remains very challenging, the preparation of fluoranthenes from 1,8-dibromonaphthalene via Suzuki coupling followed by intramolecular C–H activation has also been investigated to provide a complementary method. Using the most appropriate synthetic route and substrates, it is possible to introduce the desired functional groups at positions 7–10 on fluoranthenes.

This study aimed to evaluate Pinus halepensis Mill. seeds oil as well as methanolic‐aqueous extract on fatty acid and phenolic's composition as well as antioxidant activities with regard to the cones drying methods: convection and sun methods. The highest amounts of total phenols (14.63 ± 0.05 mg GAE/g DW), flavonoids (3.3 ± 0.02 mg QE/g DW), and condensed tannins (0.36 ± 0.05 mg CE/g DW) were showed in the seeds obtained by sun‐dried method. Methanolic‐aqueous seeds extracts were subjected to LC‐ESI‐MS analysis in order to identify and quantify the phenolic composition. This technique allowed us to identify eleven phenolic compounds: two phenolic acids and nine flavonoid compounds such as cirsiliol, catechin (+), luteolin, and luteolin‐7‐O‐glucoside, which were present in the two studied samples while apigenin, naringenin, and cirsilineol were only identified in the extract obtained from sun‐drying method seeds. The chemical components of the oils were analyzed using GC, and significant differences were found between the two studied seeds oil (p < .05). Furthermore, the antioxidant activities were investigated using DPPH and ABTS.+ assays. The results showed that the methanolic‐aqueous extract from seeds dried by sun method had the highest antioxidant activities (0.08 and 0.05 mg/ml, respectively). This study could provide useful information for industry to produce potentially bioactive plant extract. Minirel contents of Pinus halepensis Mill. seeds were present in significant amounts and very rich in K, Na, Ca and Fe. On the other hand, cirsiliol, catechine (+), luteolin and luteolin‐7‐O‐glucoside were present in the two studied samples while apeginin, naringenin and cirsilineol were only identified in the extract obtained from sun drying method seeds’. These results may be attractive for various commercial purposes as food supplements and herbal medicine products.

The extraction of the total soluble solid compounds from the pulp fruit Phoenix dactylifera L. is a major challenge for their valorization in the date fruit industry. However, conventional aqueous extraction methods are limited in terms of efficiency and processing time. In order to optimize this process, this study explores and compares three extraction methods: microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), and conventional water bath–assisted extraction (WAE). The primary objective of this study is to maximize extraction recovery (ER) by performing an optimization using a Box–Behnken design (BBD). The second objective is to analyze the impact of the three extraction methods on extraction recovery, functional attributes, biochemical characteristics, antioxidant and antibacterial activities of the optimized date pulp aqueous extract (DPAE). Results obtained using mathematical models showed significant differences (p < 0.05) between the three methods tested. Optimum extraction conditions were determined as follows: for WAE, a solid/liquid (S/L) ratio of 1/4.68 g/mL, a temperature of 80 ℃, and a duration of 38.63 minutes; for MAE, an S/L ratio of 1/6 g/mL, an irradiation power of 480 W, and a duration of 11 minutes; for UAE, an S/L ratio of 1/5 g/mL, a sonication amplitude of 40%, and a duration of 60 minutes. The MAE method stood out for its extraction efficiency, with ER = 79.90% ± 1.54% and being three times faster than WAE and MAE. It also provided the highest concentrations of total soluble solids (14.33% ± 0.11% FW), total sugars (22.23 ± 0.23 g/100 mL DPAE), and total polyphenols (1.69 ± 0.04 mg GAE/mL DPAE). The antioxidant activity of DPAE was high, with an IC50 of 729.80 ± 12.87 μg/mL of the methanolic extract. These results suggest that the optimization of extraction processes, particularly using microwave technology, could offer promising prospects for the valorization of date fruit products by improving the production efficiency of a natural and nutritious DPAE, potentially beneficial to the date fruit industry in terms of product quality and cost reduction.

In this work, spent coffee grounds (SCG) were treated using sulfuric acid hydrolysis in order to isolate the sulfuric acid lignin (SAL). The reactivity of SAL was improved through phenolation and acetylation. Spectroscopic analysis showed that the isolated lignin is composed of GHS type and it was characterized by a high amount of (C–C) and β-O-4 bonds. The thermal analysis showed that the phenolated sulfuric acid lignin (Ph-SAL) present higher thermal stability compared to SAL and acetylated sulfuric acid lignin. In addition, the phenolic hydroxyl group content increases from 2.99 to 9.49 mmol/g after phenolation. Moreover, a methylene blue (MB) adsorption test was established in order to find out the sorption capacity of different samples. The study showed that the adsorbed amount of dye increase after the chemical modification of SAL, especially after phenolation. The removal efficiency was enhanced after modification to reach 99.62% for Ph-SAL. The evaluation of the adsorption experimental data with the theoretical models of Langmuir and Freundlich showed that the best fitting was expressed by the Langmuir model for all samples. Finally, this study showed that lignin isolated from SCG can be simply and easily chemical modified and exhibits excellent adsorption ability towards cationic dyes (MB) in aqueous solutions. As a renewable, low-cost, and natural biomass material, lignin from SCG shows a promising practical and economical application of biomass in the field of wastewater purification.

The aim of this work is to investigate the adsorption of an anionic dye, the Murexide (MX) present in aqueous solution, on activated carbon, derived from prickly pear seed cake biomass after bio-oil extraction. The obtained adsorbent used was characterized by Bohem titration, pH of point of zero charge (pHPZC), FTIR spectroscopy, Brunauer–Emmett–Teller surface area (SBET), and scanning electron microscopy (SEM). The different experimental parameters of the adsorption process, such as temperature, contact time, initial dye concentration, and adsorbent dose, were studied. For the optimization of the process, the effects of these parameters were investigated using the full factorial experimental design methodology. Design Expert 11.1.2.0 Trial software was used for generating the statistical experimental design and analysing the observed data. Langmuir and Freundlich’s adsorption models were employed to provide a description of the equilibrium isotherm. The adsorption process was found to obey Langmuir, which indicates that the Murexide had formed a monolayer onto activated carbon. Furthermore, according to the regression coefficients, it was observed that the kinetic adsorption data can fit better by the pseudo-second-order model compared to the first-order Lagergren’s model. The thermodynamic studies indicated that the adsorption of Murexide occurs in a spontaneous and exothermic process. The regeneration process of the exhausted adsorbent was studied to assess the economic and operational feasibility. According to the obtained findings, it is proposed that the activated carbon prepared from prickly pear seed cake retains a high potential for Murexide removal and is suitable for repetitive usage.

The reactivity of 2-bromo- and 2,5-dibromoselenophenes in Pd-catalyzed direct heteroarylation was investigated. From 2-bromoselenophene, only the most reactive heteroarenes could be employed to prepare 2-heteroarylated selenophenes; whereas, 2,5-dibromoselenophene generally gave 2,5-di(heteroarylated) selenophenes in high yields using both thiazole and thiophene derivatives. Moreover, sequential catalytic C2 heteroarylation, bromination, catalytic C5 arylation reactions allowed the synthesis of unsymmetrical 2,5-di(hetero)arylated selenophene derivatives in three steps from selenophene.

In this study, we evaluated the use of prickly pear seed cake, a by-product of prickly pear seed oil extraction, as a new precursor for producing activated carbon by phosphoric acid activation, and the obtained carbon’s capacity for heavy metal removal from aqueous solution. Response surface methodology based on the full factorial design at two levels (24) was developed to reduce the number of experiments and reach optimal preparation conditions for the removal of cadmium and lead ions from aqueous solutions. Design Expert 11.1.2.0 Trial software was used for generating the statistical experimental design and analyzing the observed data. Factors influencing the activation process, such as carbonization temperature, activation temperature, activation time, and impregnation ratio, were studied. Responses were studied in depth with an analysis of variance to estimate their significance. Each response was outlined by a first-order regression equation demonstrating satisfactory correspondence between the predicted and experimental results as the adjusted coefficients of correlation. Based on the statistical data, the best conditions for the removal of heavy metals from aqueous solution by the obtained activated carbon were indicated. The maximum iodine number and methylene blue index were 2527.3 mg g−1 and 396.5 mg g−1, respectively, using activated carbon obtained at the following conditions: Tc = 500 °C, Ta = 500 °C, impregnation ratio = 2:1 (g H3PO4: g carbon), and activation time of two hours. The maximum adsorption reached 170.2 mg g−1 and 158.4 mg g−1 for Cd2+ and Pb2+, respectively, using activated carbon obtained at the following conditions: Tc = 600 °C, Ta = 400 °C, impregnation ratio = 2:1 (g H3PO4: g carbon), and activation time of one hour. The activated carbon obtained was characterized by Boehm titration, pH of point of zero charge (pHPZC), Brunauer–Emmett–Teller surface area (SBET), and scanning electron microscopy. Adsorption was performed according to different parameters: pH solution, adsorbent dosage, temperature, contact time, and initial concentration. Regeneration experiments proved that the obtained activated carbon still had a high removal capacity for Cd2+ and Pb2+ after five regeneration cycles.

Green chemistry focuses on reducing the environmental impacts of chemicals through sustainable practices. Traditional methods for extracting bioactive compounds from Eucalyptus marginata leaves, such as hydro-distillation and organic solvent extraction, have limitations, including long extraction times, high energy consumption, and potential toxic solvent residues. This study explored the use of supercritical fluid extraction (SFE), pressurized liquid extraction (PLE), and gas-expanded liquid (GXL) processes to improve efficiency and selectivity. These techniques were combined in a single mixture design, where CO2 was used in the experiments carried out under SFE, while water and ethanol were used for the PLE and GXL experiments by varying the concentration of the solvents to cover all the extraction possibilities. The neuroprotective activity of the extracts was evaluated by measuring their antioxidant, anti-inflammatory, and acetylcholinesterase inhibition properties. The optimization resulted in a novel GXL extraction with an optimal ternary mixture of 27% CO2, 55% ethanol, and 18% water, with a high degree of desirability (R2 = 88.59%). Chromatographic analysis carried out by GC-MS and HPLC-ESI-MS/MS identified over 49 metabolites. The designed sustainable extraction process offers a promising approach for producing phenolic-rich plant extracts in industrial applications.

Mint species (Lamiaceae family) have been used as traditional remedies for the treatment of several diseases. In this work, we aimed to characterize the biological activities of the total phenolic and flavonoid contents of Mentha pulegium L. extracts collected from two different regions of Tunisia. The highest amounts of total phenols (74.45 ± 0.01 mg GAE/g DW), flavonoids (28.87 ± 0.02 mg RE/g DW), and condensed tannins (4.35 ± 0.02 mg CE/g DW) were found in the Bizerte locality. Methanolic leaf extracts were subjected to HPLC-UV analysis in order to identify and quantify the phenolic composition. This technique allowed us to identify seven phenolic compounds: two phenolic acids and five flavonoid compounds, such as eriocitrin, hesperidin, narirutin, luteolin, and isorhoifolin, which were found in both extracts with significant differences between samples collected from the different regions (p < 0.05). Furthermore, our results showed that the methanolic extract from leaves collected from Bizerte had the highest antioxidant activities (DPPH IC50 value of 16.31 μg/mL and 570.08 μmol Fe2+/g, respectively). Both extracts showed high radical-scavenging activity as well as significant antimicrobial activity against eight tested bacteria. The highest antimicrobial activities were observed against Gram-positive bacteria with inhibition zone diameters and MIC values ranging between 19 and 32 mm and 40 and 160 µg/mL, respectively. Interestingly, at 10 μg/mL, the extract had a significant effect on cell proliferation of U87 human glioblastoma cells. These findings open perspectives for the use of Mentha pulegium L. extract in green pharmacy, alternative/complementary medicine, and natural preventive therapies for the development of effective antioxidant, antibacterial, and/or antitumoral drugs.

Changes in quality parameters of flavored/aromatized Chemlali olive oil by the green addition of Verbena officinalis L. phenolic-rich extract were studied as a function of storage time (6 months) at room temperature (20 °C). Evaluation of oil quality was established by studying the FA, PV, K 232 , K 270 parameters, as well as chlorophyll and carotenoid contents, total phenolic and flavonoid content (TPC and TFC, respectively). Results showed that chlorophyll and carotenoid pigments decomposed, respectively, for more than 30 and less than 24% in the flavored/aromatized oil samples stored at 20 °C. Additionally, the decreasing rate of phenolic and flavonoid content in the flavored olive oil was lower than that in the control samples. These findings proved that aromatization with Verbena officinalis L. phenolic-rich extract obtained after optimisation of microwave parameters may be an alternative to improve olive oil quality and create a new competitive flavored product.