(3) Compound 1 in the attached paper is very similar to [Mn(III)(salpn)(H2O)2](C
ID: 939907 • Letter: #
Question
(3) Compound 1 in the attached paper is very similar to [Mn(III)(salpn)(H2O)2](CF3SO3) you made today. Why did’t we use HClO4/H2O instead of triflic acid for the synthesis?
http://pubs.acs.org/doi/abs/10.1021/ja00010a025?journalCode=jacsat
Experiment Guide:
[MnIII(salpn)(H2O)2](CF3SO3) In a round bottom flask, to a slurry of 1.5 mmoles MnIII(salpn)(AcAc) (0.65 g) in 15 mL of acetonitrile, add 1.5 mmol of trifluoromethanesulfonic acid (triflic acid, 1.5 ml of a 1.0 M solution in acetonitrile) dropwise.
• Stir 15 minutes, filter if some solid remains, then reduce solvent to about 5 ml by rotary evaporation (do not reduce the solvent too much).
• Transfer concentrated solution/slurry to a 100-250 mL beaker. • Add about 25 ml ether to the solution and collect the solid by vacuum filtration.
• When it is dry, determine the yield.
Explanation / Answer
The addition of strong acid like triflic acid is important to this reaction because you need very strong acid to replace the acac ligands attached to manganese. Since perchlorate is weak acid to favor this ligand exchange, so you will not end with the desire product.
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