The effectiveness of microwave-assisted synthesis of 5,10,15,20-tetraphenylporphyrin and its corresponding to metal complexes of (Bi (III), Zn (II) and Ni (II)) are described. Moreover, the synthesized metalloporphyrins that were obtained with reasonable yields were characterized using UV-vis, 1 H-NMR and IR.
Organic synthetic research laboratories generate a large amount of waste. Some of the waste is the silica gel used as the stationary phase in column chromatographic separations. Here, the authors discuss the possibility of recycling silica gel wastes thermally at 600 °C, at which temperature the remnant adsorbed organic material combusts. It could be shown that the recycled silica gel maintains its adsorption characteristics. The process could be repeated 10 times with any discernable deterioration of the separation properties of the silica gel for the product mixture of the reactions used in this research. In those cases where triphenyl oxide remained on the silica gel after the separation of the reaction mixture, such as after Wittig olefination and Appel-type reactions, an increase of phosphorus content was noted in the silica gel after thermal treatment. The original and recycled silica gel was partly analyzed by Brunauer-Emmett-Teller (BET) surface measurements, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and in inductively coupled plasma optical emission spectroscopy (ICP-OES). The process significantly reduced waste production in our laboratory and also led to a reduction in costs associated with acquiring new silica gel and with the management and the disposal of spent silica gel. A simple environmental impact assessment has been carried out.
Activated alkenes such as cinnamates and chalcones can easily be converted to 2,3-dideuterio-arylpropionates and dideuteriochalcones, respectively, by the action of NaBD4, AcOD in the presence of Pd on carbon. Toluene or benzene was used as solvent. It was shown that Pd on carbon was necessary for the reaction to proceed. Deuterium addition experiments were also carried out with NaBD4, AcOD, D2O in the presence of Pd on carbon.
Abstract:The Appel reaction of an alcohol with CCl4/PPh3 and with CBr4/PPh3 produce alkyl chlorides and alkyl bromides, respectively. It was found that in the case of using BrCCl3-PPh3, a mixture of alkyl chlorides and alkyl bromides are formed. Dichloromethane (CH2Cl2) and acetonitrile (CH3CN) were used as solvents, where the reaction was found to be solvent-dependent.
The guest-host interaction between Dapsone drug and β-cyclodextrin (β-CD) was investigated using fluorescence spectroscopy, 1 H-NMR, and liquid chromatography with fluorescence detection. The optimized conditions for the interaction were investigated by spectrofluorometry and were found to be at 0.2 mg/mL (0.176 mM) of β-CD and pH 8.8. For these conditions, very low concentration of Dapsone drug of 2.4 ng/mL (12.97 nM) can be detected. The standard addition method was utilized to detect Dapsone in influent and effluent wastewater samples in the sub parts per billion concentration range by HPLC-FLD using β-CD as an additive in the mobile phase.
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