Abstract: Bimolecular L-valine hydridophosphorane was synthesized by the reaction between L-valine and phosphorus trichloride in tetrahydrofuran (THF). Complete assignment of the ¹³C NMR chemical shifts of the compound was obtained by 2D NMR techniques, including ¹H-¹H COSY, DEPT and HSQC. Based on the results of NMR characterization, the structure of L-valine hydridophosphorane was elucidated. The ³¹P NMR spectrum of the compound showed two separated peaks at δ -64.66 and δ -67.81, suggesting that it is comprised of a pair of diastereomers. The configuration of one of the diastereomers was determined by NOESY, and further confirmed by X-ray crystallography.

Key words: NMR, assignments, configuration, valine hydridophosphorane