Ru-catalyzed synthesis of substituted phthalides through C–H bond activation and functionalization

Synthesis of substituted phthalides through a ruthenium-catalyzed reaction of phthalic anhydrides with acrylates is described. The reaction proceeds via CH bond activation and leads to the formation of vinylated phthalides through a successive double vinylation accompanied by decarboxylation and annulation reactions.     

Experimental and Theoretical Study of the Effect of Moisture on Methane Adsorption and Desorption by Activated Carbon at 273.5 K

Adsorption and desorption of methane by activated carbon (AC) at constant temperature and at various pressures were investigated. The effect of moisture was also studied. A volumetric method was used, up to 40 bar, at a temperature of 273.5 K. Results of a dry AC sample were compared with those obtained from a moist sample and two different ACs with different physical and surface properties were used. As expected, the results showed that the existence of moisture, trapped in the AC pores, could lead to a decrease in the amount of methane adsorbed and a decrease in the amount of methane delivered during desorption. To model the experimental results, a large variety of adsorption isotherms were used. The regressed parameters for the adsorption isotherms were obtained using the experimental data generated in the present study. The accuracy of the results obtained from the different adsorption isotherms was favorably compared.     

Nano-Fe3O4-encapsulated silica particles bearing sulfonic acid groups as a magnetically separable catalyst for green synthesis of 1,1-diacetates

Sulfonic acid-functionalized silica-coated nano-Fe₃O₄particles (Fe₃O₄@SiO₂–SO₃H) serve as a novel heterogeneous catalyst for the synthesis of acylals by direct condensation of aldehydes with acetic anhydride under solvent-free conditions at room temperature in short reaction times and excellent yields. The catalyst could be easily separated from the final product using an external magnet and reused several times without consequential loss of reactivity.     

A three‐phase solvent extraction system combined with deep eutectic solvent‐based dispersive liquid–liquid microextraction for extraction of some organochlorine pesticides in cocoa samples prior to gas chromatography with electron capture detection

A sample pretreatment method based on the combination of a three‐phase solvent extraction system and deep eutectic solvent‐based dispersive liquid–liquid microextraction has been introduced for the extraction of four organochlorine pesticides in cocoa samples before their determination by gas chromatography‐electron capture detection. A mixture of sodium chloride, acetonitrile, and potassium hydroxide solution is added to cocoa bean or powder. After vortexing and centrifugation of the mixture, the collected upper phase (acetonitrile) is removed and mixed with a few microliters of N,N‐diethanol ammonium chloride: pivalic acid deep eutectic solvent. Then it is rapidly injected into deionized water and a cloudy solution is obtained. Under optimum conditions, the limits of detection and quantification were found to be 0.011‐0.031 and 0.036‐0.104 ng/g, respectively. The obtained extraction recoveries varied between 74 and 92%. Also, intra‐ (n = 6) and interday (n = 4) precisions were less than or equal to 7.1% for the studied pesticides at a concentration of 0.3 ng/g of each analyte. The suggested method was applied to determine the studied organochlorine pesticide residues in various cocoa powders and beans gathered from groceries in Tabriz city (Iran) and aldrin and dichlobenil were found in some of them.     

Development of a stir bar sorptive extraction method coupled to solidification of floating droplets dispersive liquid–liquid microextraction based on deep eutectic solvents for the extraction of acidic pesticides from tomato samples

A stir bar sorptive extraction method coupled with deep eutectic solvent based solidification of floating organic droplets–dispersive liquid–liquid microextraction has been used for the simultaneous derivatization and extraction of some acidic pesticides in tomato samples. In this method, initially the analytes are adsorbed on a coated stir bar from tomato juice filled in a narrow tube. After extraction, the stir bar is removed and a water–miscible deep eutectic solvent is used to elute the analytes. Afterward, a derivatization agent and a water–immiscible deep eutectic solvent (as an extraction solvent) with melting point near to room temperature are added to the obtained eluant at µL–levels and the obtained mixture is rapidly injected into deionized water. Under the optimum conditions, the introduced method indicated high enhancement (1543–3353) and enrichment (2530–2999) factors, low limits of detection (7–14 ng/L) and quantification (23–47 ng/L), good linearity (r² ≥ 0.9982), and satisfactory repeatabilities (relative standard deviation ≤12% for intra– and inter–day precisions at a concentration of 100 ng/L of each analyte). Finally, the proposed method was applied in analysis of the analytes in tomato samples.