Compound 5
(R,R)-Mn(PDP)(MeCN)2(SbF6)2
From: Chemoselective methylene oxidation in aromatic molecules
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Compound data: Crystallographic data
Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.
In a flamed dried 100 mL recovery flask was charged (R,R)-Mn(PDP)Cl2 S1 (1.2073 g, 2.69 mmol), a stir bar and 35 mL anhydrous MeCN. AgSbF6 (purchased from Strem, 1.8508 g, 5.39 mmol, 2.0 equiv.) was weighed under argon atmosphere in glove box and then added to the reaction under a stream of nitrogen. The flask was wrapped with aluminum foil to protect from light and the reaction was vigorously stirred for 24 hours. AgCl precipitated out and the reaction was filtered through a pad of Celite® and concentrated under vacuum to a minimum amount of MeCN remaining. The residue was redissolved in a minimum amount of MeCN and filtered through a 0.22 μm Acrodisc® LC PVDF filter (HPLC certified) and concentrated. The filtration-concentration process was repeated two more times and the residue was concentrated to a minimum amount of MeCN remaining and then dried under a positive stream of nitrogen for 24 hours. (R,R)-Mn(PDP)(MeCN)2(SbF6)2 5 was obtained as a white solid (2.3795 g, 2.56 mmol, 95% yield). HRMS (TOF ESI+) m/z calculated for C20H26N4F6MnSb [M-SbF6-2(MeCN)]+: 612.0480, found 612.0469.
