Boekelheide reaction explained

The Boekelheide reaction is a rearrangement of α-picoline-N-oxides to hydroxymethylpyridines. It is named after Virgil Boekelheide who first reported it in 1954.[1] Originally the reaction was carried out using acetic anhydride, which typically required a period at reflux (~140 °C). The reaction can be performed using trifluoroacetic anhydride (TFAA), which often allows for a room temperature reaction.[2]

Mechanism

The mechanism of the Boekelheide reaction begins by an acyl transfer from the trifluoroacetic anhydride to the N-oxide oxygen. The α-methyl carbon is then deprotonated by the trifluoroacetate anion. This sets the molecule up for a [3.3]-sigmatropic rearrangement which furnishes the trifluoroacetylated methylpyridine. Hydrolysis of the trifluoroacetate releases the hydroxymethylpyridine.

Notes and References

  1. Boekelheide. V.. Linn. W. J.. Rearrangements of N-Oxides. A Novel Synthesis of Pyridyl Carbinols and Aldehydes. Journal of the American Chemical Society. March 1954. 76. 5. 1286–1291. 10.1021/ja01634a026.
  2. Fontenas. C.. Bejan. E.. Haddou. H. Aït. Balavoine. G. G. A.. The Boekelheide Reaction: Trifluoroacetic Anhydride as a Convenient Acylating Agent. Synthetic Communications. 23 September 2006. 25. 5. 629–633. 10.1080/00397919508011399.