Straightforward Access to Free β2,3,3‐Amino Acids through One Pot C‐H Activation/C−C Cleavage

The first synthesis of unnatural β2,3,3‐amino acids with a spirocyclic backbone by one‐pot protocol has been presented. This reaction features wide functional group tolerance and feasibility of post‐functionalization of natural products and biologically important molecules. Novel dipeptide and tripeptide structures were assembled using this newly developed β2,3,3‐amino acid in high efficiency. The combination of C−H activation and C−C cleavage for the synthesis of β‐amino acids would trigger more promising synthetic routes for this compound. Herein, one‐pot C−H activation/C−C cleavage for the synthesis of novel spirocyclic β2,3,3‐amino acids, is reported. This approach shows wide substrate scope of CF3‐ynones and ketimines. In addition, several natural products and biologically relevant molecules, prepared by this method, can be further functionalized. Novel dipeptide and tripeptide structures can be successfully assembled with this spirocyclic amino acid.