Diphenylphosphinic chloride → P,P-Diphenylphosphinic azide

Participants

Reaction Conditions

Reaction Steps

Following a previously [Paciorek et al, Inorg. Nucl. Chem. Letters, 2, 39 (1966)] developed procedure, diphenylphosphinyl chloride (14.87 g, 62.86 mmol) was introduced into a tube (in the inert atmosphere enclosure). Trimethylsilyl azide (10.45 g, 90.69 mmol) was then condensed onto this material on a vacuum line at liquid nitrogen temperature. The tube was sealed in vacuo and heated at 60° C. for 48 hr. Thereafter, it was cooled, opened to a vacuum system and the volatiles were collected in a liquid nitrogen trap (originally without pumping at room temperature, finally with pumping at 70° C.). The total time required to remove the volatiles (excess (CH3)3SiN3 and the by-product (CH3)3SiCl) was 16 hr. A quantitative yield of pure diphenylphosphinyl azide was realized.

Provenance & Evidence