Argon-purged dichloromethane

Room temperature argon-purged dichloromethane solution and reversible and monoelectronic processes, unless otherwise noted tetrabutylammonium hexafluorophosphate as supporting electrolyte, glassy carbon as working electrode. bPurified tetrahydrofurane under vacuum conditions. Irreversible process potential value estimated by the DPV peak. 

In the electrochemical experiments performed in argon-purged dichloromethane solution, [Os(bpy)2(l)]2+ undergoes a reversible monoelectronic oxidation at +1.03 V vs SCE (Figure 7, Table 2), that can be assigned to the oxidation of Os(II)[6c,e]. The potential value at which the metal ion is oxidized is very close to those obtained for the metal oxidation in the model compounds [Os(bpy)2(5)]2+ and [Os(bpy)3]2+ (Table 2). On reduction, two reversible and monoelectronic processes are observed in the accessible potential window (Figure 7, Table 2). 

Figure 7. Cyclic voltammogram obtained for [Os(bpy)2(l)]2+ complex (argon-purged dichloromethane complex concentration 4 x llL1 M glassy carbon as working electrode, scan rate of 100 mV/s).

The electrochemical investigation of ligands 1, 2, 5 and bpy was carried out by using the equipment and procedure previously described [8], The equipment 19] and procedure [8] used for investigation of the electrochemical behavior of the complexes in argon-purged Hi-diy dichloromethane have been previously described. 

Reduction of 2,2-bisf3 -nltro-4 -(4"-phenylsulfonylphenoxyl)phenyl1 propane. Compound 9, 200 mg (0.55 meg) was dissolved in a mixture of 30 mL of dichloromethane (DCM) and 30 mL of methanol and 240 mg of 10% palladium on charcoal was added. After purging the solution with argon for 30 min, 520 mg (13.6 mmol) of sodium borohydride was added portionwise over 10 min. The reaction mixture was stirred under argon for 1 hr before addition of 30 mL of DCM. The mixture was filtered, the filtrate evaporated, and the residue extracted with DCM. Evaporation of the extract yielded 140 mg (76.2%) of 2,2-... 

A. N-(2-Benzoyl-4-chlorophenyl)oxanilic acid ethyl ester. A two-necked, round bottomed flask (500 mL) equipped with a Teflon-coated magnetic stirring bar, a ga9 inlet, and a dropping funnel is purged with argon. The flask is charged with 2-amino-5-chlorobenzophenone (13.9 g, 60 mmol, Note 1), dichloromethane (100 mL), and pyridine (20 mL, Note 2). A solution of ethyl oxalyl chloride (9.6 g, 70.3 mmol, Note 1)... 

Peanut Oil/Cysteine and Peanut Oil/Methionine Systems. Peanut oil (100 g) and 10.0 g of cysteine or methionine were mixed and placed in a 500-mL two-neck round-bottom flask, which was interfaced to a simultaneous purging and solvent extraction (SPE) apparatus developed by Umano and Shibamoto 13). The mixture was heated at 200 C for 5 hr while stirring. The headspace volatiles were purged into 250 mL of deionized water by a purified nitrogen stream at a flow rate of 10 mL/min. The volatiles trapped by the water were continuously extracted with dichloromethane (50 mL) for 6 hr. The water temperature was kept at 10°C by a Brinkman RM6 constant-temperature water circulator. The dichloromethane extract was dried over anhydrous sodium sulfate, and the extract was then concentrated to 2.0 mL by fractional distillation with a Vigreux colunm at atmospheric pressure. The concentrated extract was placed in a vial and stored under argon at -4 C until tested for antioxidative activity. 

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