Phosphorus trichloride and hexamethylphosphorus triamide react with N-t-butyl-2,2'-iminodiethanol (4) forming the 2 : 3 adduct N,N-bis[2-(6-t-butyl-l,3,6,2-dioxazaphosphoran-2-yloxy)ethyl-t-butylamine (5) which, on treatment with water (2 mol equiv.) is hydrolysed to give 6-t-butyl-1,3,6,2dioxazaphosphocane 2-oxide (8) and N-t-butyl-2,2'-iminodiethanol (4). Compound (8) reacts with ochloranil to produce a crystalline product which in solution gives an equilibrium mixture of six-coordinated phosphorus with a P-OH bond (9) and the phosphate ester (10). Phenylphosphonous dichloride and N,N,N',N'-tetramethyl-P-phenylphosphonous diamide react with (4) to give 2-phenyl-6t-butyl-l,3,6,2-dioxazaphosphocane (1 1 ) which adds to o-chloranil to form a tautomeric equilibrium mixture of the four-co-ordinate and six-co-ordinate phosphorus compounds (1 3) (1 4). Phenyl azide reacts with (1 1 ) to give 2-phenyl-2-phenylimino-6-t-butyl-l,3,6,2-dioxazaphosphocane (1 5). The structural assignments are based on analytical, chemical, and spectroscopic results.
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