Tetrakis triethyl phosphite nickel O

TETRAKIS(TRIETHYL PHOSPHITE)NICKEL(O), PALLADIUM(0), AND PLATINUM(O) COMPLEXES 

The triethyl phosphite (Eastman) used in these preparations was distilled in a vacuum prior to use, b.p. 51° at 13 mm. Hg. The preparations were carried out in air an inert atmosphere was not necessary. 

The nickel(0) compound can be prepared by the method of Vinal and Reynolds.1 Nickel(II) chloride hexahydrate (5.0 g., 0.021 mole) is dissolved in 100 ml. of methanol contained in a 250-ml. round-bottomed flask. A stirring bar is placed in the flask, and it is put in an ice-water bath standing on a magnetic stirrer. The solution is allowed to cool with stirring for 10 minutes, and 18 ml. of triethyl phosphite are then added over a 

Tetrakis(triethyl phosphite)nickel(0) can be handled in air. It is best stored in an evacuated and sealed tube. On exposure to air for several hours the substance turns green. The compound is insoluble in water, somewhat soluble in methanol, and very soluble in hydrocarbons. It does not dissociate in hydrocarbon solutions. 

The dry product, [Pd P(OC2H6)3 4], containing no adsorbed triethyl phosphite is air-sensitive, turning black on exposures 

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