Bis Diethylphosphinomethyl Methylamine

All reactions are performed under an inert atmosphere using standard Schlenk techniques, and all solvents are dried and degassed by standard procedures before use. Starting materials are reagent-grade commercially available compounds, with the exception of [Ni(MeCN)6] (BF4)2-0.5MeCN, which is prepared by a previously reported procedure.10 

A 250-mL Schlenk flask is charged with diethylphosphine (2.27 g, 25.2 mmol) and degassed aqueous formaldehyde (37wt%, 1.95 mL, 26 mmol) in ethanol (10 mL), and the solution is stirred for 30 min. A solution of hydrochloride salt of methylamine (MeNH3Cl, 0.85 g, 12.65 mmol) in an ethanol/water solution (10 mL, 3 1 ratio) is added by cannula or syringe to the phosphine solution. Finally, triethylamine (2 mL, 14 mmol) is added to deprotonate the methylamine salt. The 

The PNP ligand is an air-sensitive, clear high-boiling liquid that is soluble in most organic solvents. It can be characterized by its H and 31P NMR spectra. 

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