Abstract
The condensation reactions of partly substituted spiro-cyclotriphosphazenic lariat (PNP-pivot) ethers, N 3P 3[( o-NHPhO) 2R]Cl 4 [where R = –CH 2CH 2– ( 1) and –CH 2CH 2OCH 2CH 2– ( 2)] with morpholine and 1,4-dioxa-8-azaspiro[4,5]decane (DASD) produce fully substituted morpholino ( 3 and 4) and 1,4-dioxa-8-azaspiro[4,5]deca ( 5 and 6) phosphazenes. These are the new examples of the spiro-cyclophosphazenic lariat ether derivatives with N 2O x ( x = 2 and 3) donor type containing 11- and 14-membered macrocycles. The solid state structures of 3, 5 and 6 have been determined by X-ray diffraction techniques. Compound 3 has intermolecular N–H…O hydrogen bond, compound 5 has intra- and intermolecular N–H…O hydrogen bonds, while compound 6 has intramolecular N–H…O and O–H…N and intermolecular N–H…O and O–H…O hydrogen bonds. The correlations of the endocyclic ( α) and exocyclic ( α′) NPN bond angles with δP spiro values are investigated. The structural investigations of 3– 6 have been verified by elemental analyses, MS, FTIR, 1H, 13C and 31P NMR, DEPT and HETCOR techniques.
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