Synthesis and Structure Studies of Complexes of Some Second Row Transition Metals with 1-(Phenylacetyl and Phenoxyacetyl)-4-phenyl-3-thiosemicarbazide
| Autor: | Sahar I. Mostafa, M. M. Bekheit |
|---|---|
| Rok vydání: | 2000 |
| Předmět: |
Thiosemicarbazones
chemistry.chemical_classification Differential Thermal Analysis Magnetic Resonance Spectroscopy Aqueous solution Ketone Spectrophotometry Infrared Silica gel Stereochemistry Sodium periodate Electric Conductivity General Chemistry General Medicine Aldehyde Catalysis chemistry.chemical_compound chemistry Metals Drug Discovery Acetone Anhydrous Spectrophotometry Ultraviolet Diethyl ether Oxidation-Reduction Nuclear chemistry |
| Zdroj: | Chemical and Pharmaceutical Bulletin. 48:266-271 |
| ISSN: | 1347-5223 0009-2363 |
| DOI: | 10.1248/cpb.48.266 |
| Popis: | (0.087 g, 0.5 mmol) in H2O (1 ml) was added to H2papts (0.143 g, 0.5 mmol) or H2pxapts (0.151 g, 0.5 mmol) in EtOH (10 ml) to give yellow (H2papts) or orange-brown (H2pxapts) solids. These were left in the dark for 3 h, filtered off, washed with little H2O, EtOH, Et2O and dried in the dark in vacuo. Trans-[UO2(HL)(bipy)(AcO)(H2O)2 ]· nH2O (HL5Hpapts, n53; HL5 Hpxapts, n50; bipy52,29-bipyridyl): Hydrated uranyl acetate (0.21 g, 0.5 mmol) in MeOH (10 ml) was added to a MeOH solution of 2,29-bipyridyl (0.078 g, 0.5 mmol) and H2papts (0.143 g, 0.5 mmol) or H2pxapts (0.151 g, 0.5 mmol). The resulting solution was boiled under reflux for 3 h in a steam bath. The red-orange (H2papts) or yellow (H2pxapts) solutions were reduced in volume until the precipitates separated out. These were filtered off, washed with little MeOH and dried in a desicator over silica gel. [Ag(H2papts)(bipy)]BPh4: AgNO3 (0.087 g, 0.5 mmol) in H2O (0.5 ml) was added to 2,29-bipyridyl (0.078 g, 0.5 mmol) in MeOH (25 ml) to form a colorless solution, to which H2papts (0.143 g, 0.5 mmol) in MeOH (10 ml) was added to produce a red-brown solution. NaBPh4 (0.17 g, 0.5 mmol) in MeOH (5 ml) was added and the precipitate was separated out. This was filtered off, washed with a little H2O, MeOH, Et2O and dried in the dark in vacuo. [Pd(Hpapts)(bipy)]BPh4: The complex [Pd(bipy)Cl2] was prepared by the literature method. 12) To a stirred suspension of [Pd(bipy)Cl2] (0.17 g, 0.5 mmol) in acetone (10 ml), H2papts (0.143 g, 0.5 mmol) and KOH (0.056 g, 1 mmol) in MeOH (10 ml) was added. The mixture was stirred overnight. NaBPh4 (0.17 g, 0.5 mmol) in MeOH (5 ml) was added to the resulting brown solution. The complex was filtered off, washed with MeOH, Et2O and dried in vacuo. Catalytic Oxidation For the catalytic oxidation by [Ru(HL)2(H2O)2] (HL5Hpapts, Hpxapts) complexes, the organic substrate (1.0 mmol) was added to NaIO4 (2.5 mmol) in CCl4‐CH3CN‐H2 O (1 :1:2 ; 20ml) and the catalyst (0.02 mmol). The reaction mixture was stirred under reflux at 70 °C, then cooled and extracted with diethyl ether (3320 ml). The etheral layer was then dried with anhydrous Na2SO4 and the aldehyde or ketone content quantified as its 2,4-dinitrophenylhydrazone derivatives. The aqueous layer 266 |
| Databáze: | OpenAIRE |
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