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Abstract
Several synthetic schemes have been devised starting from [N,N-diethyl phenylphosphinamide]pentacarbonyltungsten 1. Metalation of the P[sbnd]H bond of 1 by butyllithium followed by reaction with allyl bromide afforded [N,N-diethyl allylphenylphosphinamide]pentacarbonyltungsten 3 which was treated with anhydrous HCl to get [allylphenylchlorophosphine]pentacarbonyltungsten 4. We tried without success to eliminate HCl from 4 in order to obtain [1-phenylphosphabutadiene]pentacarbonyltungsten 5. Metalation of 1 followed by reaction with p-chlorobenzaldehyde gave [N,N-diethyl(p-chlorophenyl-hydroxymethyl)phenylphosphinamide]pentacarbonyltungsten 9 which yielded [(p-chlorophenylhydroxymethyl)phenylchlorophosphine] pentacarbonyltungsten 10 by reaction with HCl. Complex 10 is stable towards the elimination of HCl and does not give the corresponding 1,2-oxaphosphirane by treatment with NaH. Metalation of 1 followed by reaction with benzoyl chloride gave the corresponding benzoylphosphinamide 12 which, when treated by HCl, afforded [benzoylphenylchlorophosphine]pentacarbonyltungsten 13. The low temperature reaction of 13 with NH3 gave [benzoylphenylphosphinamide]pentacarbonyltungsten 14. The dehydration of 14 to obtain the corresponding 1,2-azaphosphirene was unsuccessful.
