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, The TiOTPyP-H reagent (~4.5.10 -5 M) was prepared by dissolving 3.44 mg of commercial TiOTPyP complex (?90%, from TCI) in 100 mL of 0.05 M HCl and stored at 0°C. An aliquot, p.15
, The method was calibrated by replicating the same procedure using aqueous solutions of H2O2 (in the 0-5 µM range, prepared by dilution of a 0.105 M standard solution), instead of the sample solutions. The obtained ?A values (?Acal(i)) were plotted against H2O2 concentration in the final sample, the catalytic solution was added to a mixture of TiOTPyP-H (250 µL), perchloric acid (4.8M, 250 µL) and water (235 µL)
, Asample(i)) was determined. The concentration of H2O2 in the original samples (i.e. before addition to the TiOTPyP reagent solution) is determined by taking into account the dilution factor
, Note 1: 70 % of H2O2 would mean that we also produce 30 % of H2O (yield calculated against the electron quantity in solution)
, Note 2: As TiOTPyP-H reacts with Me8Fc, the titration cannot be done if all the sacrificial reducing agent is not completely consumed. 14. Verify that the pressure in the device didn't change while filling the UV cell with a solution
, Ending an experiment: 1. Stop the motor device
, Open V2 slowly to empty the device until -0.2 bars. 3. Unscrew V1
, Disconnect the needles from the UV cell
, Stop the vacuum pump
, It is further oxidized into its disulfide analog to be easier to handle and subjected to chlorination and nucleophilic substitution with the desired secondary amine to give the targeted ligands. We then envisaged to prepare dissymmetrical units (achieved through routes (A) and (B), Scheme 1) and investigated route (A) that involves the mono-reduction of the O-(2,6-diformyl-4-methylphenyl) dimethylthiocarbamate synthon (1). NaBH 4 was used as typical reducing agent of the aldehyde function
CNRS UMR 5249, CEA, 17 rue des martyrs, F-38054, Univ. Grenoble Alpes ,
Grenoble Alpes), 17 rue des Martyrs, F-38054 Grenoble Cedex 9 ,
MAM)SÀS and targeted dissymmetrical ligands. (a) DABCO, ClCSN(Me) 2 , DMF, 12 h; (b) BF 3 -Et 2 O, (ClCH 2 ) 2 , reflux, Figure 1. Conversion of (1) into (1 a) and formation of (1 b) via tandem reduction /migration of the thiocarbamate moiety ,
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