also provides a convenient route for synthesizing the dibasic 12-carboxymethyldihydroabietic acid (XII) from levopimaric acid.
Parkin, B. A., Jr., Summers, H. B., Jr., Settine, R. L., Hedrick, G. W., IND.ENG.CHEM.PROD. RES. DEVELOP. 5 , 257 (1966).
Literature Cited
Parkin, B. A., Jr., Hedrick, G. W., J . Org. Chem. 30, 2356 (1965).
RECEIVED for review December 5 , 1968 ACCEPTED February 26, 1969
NICKEL COATINGS FROM THE THERMAL DECOMPOSITION OF NICKEL(0) A LKY LPHOSPHITE SO LUT IONS D .
P .
J O R D A N
A N D
D .
H .
A N T O N S E N
Paul D. Merica Research Laboratory, T h e International Nickel Co., Inc., Sterling Forest, Suffern, N . Y . 10901 The thermal decomposition of solutions containing tetrakis( trialkylphosphite) nickel(0) compounds was studied. At 200' to 25OoC. the compounds break down into metallic nickel and free ligands. When the solutions are heated in glass tubes, nickel mirrors coating the walls are formed along with precipitated nickel powder. Under these conditions the nickel deposits always contain up to 20% of a by-product expressed as Ni,P02. When heated metal substrates are introduced into these solutions, coherent high purity nickel deposits result (99.95% pure) and plating rates of 2.0 mils per hour can be achieved.
SEVERAL classes of
zero-valent compounds are known. Among these are the tetrakis(trialky1phosphite) nickels described by Vinal and Reynolds (1963) and later by Olechowski et al, (1965). These compounds are colorless, nonvolatile, crystalline solids, somewhat sensitive to air oxidation. They exhibit solubility in polar solvents and a t elevated temperatures are somewhat soluble in high molecular weight hydrocarbons. In their preparation nickel bromide dihydrate reacts with trimethylphosphite to form hexakis(trimethy1phosphite) nickel bromide.
NiBr2.2HrO
+ G(CH3O)IP
CHICK 250 c.
[ (CH30)3P],NiBr2+ 2 H 2 0 The latter compound is then treated with base, and tetrakis(trimethy1phosphite) nickel(0) is formed along with trimethylphosphite and trimethylphosphate.
[(CH?O),P],NiBr,
+ HrO + 2EtjNH
[(CHJO),P]&i
-20"
c.
+ (CHIO)]P + (CHIO)
