Tervalent Phosphorus-Nitrogen Ring Compounds

The material so prepared is generaUy pure enough for most purposes. 

Cowley, Compounds Containing Phosphorus-Phosphorus Bonds, Benchmark Papers, Dowden, Hutchinson, and Ross Inc., Stroudsburg, PA, 1973. 

Submitted by O. J. SCHERER and R. ANSELMANN Checked by R. T. PAINEt and S. KARTHIKEYANt 

The first cyclodiphosphazane (diazadiphosphetidine) was reported by Mi-chaelis and Schroter in 1894. The synthesis of l,3-di-tert-butyl-2,4-di- 

The reaction vessel is a 2-L, three-necked flask equipped with a mechanical stirrer, a water-cooled reflux condenser, and a 1-L pressure-equalizing dropping funnel. Under inert atmosphere conditions, distilled chlorotri-methylsilane (120 mL, 102.7 g, 0.95 mol) in diethyl ether (500 mL) is added dropwise at room temperature from the dropping funnel to an efficiently stirred solution of rm-butylamine (100 mL, 69.6 g, 0.95 mol, freshly distilled from KOH) and triethylamine (135 mL, 98.2 g, 0.97 mol, freshly distilled from KOH) in diethyl ether (500 mL), The reaction mixture is stirred for 2 hr. Solid amine hydrochloride is filtered off (D3 frit) and washed twice with 100 mL of diethyl ether. Fractional distillation yields 100-120 g (70-80%), bp 119-122°/760 torr. 

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Tervalent Phosphorus-Nitrogen Ring Compounds 9 Procedure b ClPNCMe i... 

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