Phosphorus pentachloride → HCID 13037527, compound

Participants

Reaction Steps

Under anhydrous conditions, a mixture of 2-[P-ethoxy-P-methylphosphinyl]benzyl carbamic acid ethyl ester (1.2 g, 0.0025 mol) and phosphorus pentachloride (0.52 g, 0.0025 mol) in 10 ml. of carbon tetrachloride was heated at reflux for 1.5 hours. The reaction mixture was concentrated in vacuo and the resulting residue was dissolved in methylene chloride. The methylene chloride solution was washed with ice water, dried over magnesium sulfate and concentrated to produce a yellow oil. Distillation of this yellow oil at 150° C. and 0.5 torr produced an oil which solidified to yield 1-methyl-2-ethoxycarbonyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide as a white powder having a melting point of 102°-104° C. and the following analysis:

Provenance & Evidence