I require a small amount of triflic acid, and while other research groups do not have any, I did locate some trflic anhydride. Does anyone have a published protocol for obtaining the anhydrous acid from the anhydride?
I tried to distill under a slow stream of nitrogen about 10 mL of triflic anhydride (yellow/brown solution) with about 5 mL of DI H2O. I got a clear colorless fraction coming off with B.P. 66 C, and afterwards a second fraction with a slightly lower boiling point. The boiling point of the free acid is 162C, the anhydride is 82 C, and there is a monohydrate of the free acid with a melting point of 34 C, but I couldn't find the boiling point.
I did not find an entry in Perrin & Armarego Purification 3rd edition, or in my Fieser and Fieser.
I'll run 19F NMR on the 2 distilled fractions I got, but as the BP was so low, I expect not to get the free acid.