Improved Yields of Dichlorobis(triphenylphosphine)nickel(II) and Related Compounds by Employing Triethyl Orthoformate as an In Situ Dehydrating Agent: Rational Improvement of a Classic Undergraduate Inorganic Synthesis

The addition of a small excess of triethyl orthoformate to an alcoholic mixture of NiCl2.6H(2)O and triphenylphosphine (PPh3) results in an increase in the typical isolated yield of [NiCl2(PPh3)(2)] from below 50% to over 85%. The impact of water when present in the reaction medium in this system is discussed, and results from the application of the same synthetic approach to the syntheses of [NiBr2(PPh3)(2)], [NiCl2(dppe)], and [NiBr2(dppe)] are presented. A simple synthesis of NiCl2.2H(2)O by the dehydration of NiCl2.6H(2)O at 80 degrees C can be performed as an optional step to decrease the quantity of triethyl orthoformate required for the preparation of [NiCl2(PPh3)(2)] and/or [NiCl2(dppe)]. The experiments are flexible and accommodate a variety of laboratory schedules and student skill levels. Each synthesis can be readily completed within a 3 h laboratory period.

Automated summary

The addition of a small excess of triethyl orthoformate to the reaction mixture of NiCl2.6H(2)O and triphenylphosphine (PPh3) in ethanol significantly increases the yield of [NiCl2(PPh3)(2)] from below 50% to over 85%. The impact of water on the reaction system is discussed, and similar syntheses of [NiBr2(PPh3)(2)], [NiCl2(dppe)], and [NiBr2(dppe)] are presented. A simplified synthesis of NiCl2.2H(2)O by dehydration of NiCl2.6H(2)O at 80 degrees C can be performed to reduce the amount of triethyl orthoformate required for the preparation of [NiCl2(PPh3)(2)] and/or [NiCl2(dppe)]. The experiments are flexible and can accommodate various laboratory schedules and student skill levels, with each synthesis achievable within a 3-hour lab period.