Studies On Synthesis Of Aza-bridged Calix[4]arene And It's Derivation Complex With RDX And HMX

In this paper,we synthesized aza-bridged calix[4]arene and its derivation.Andstudied supramolecular complex with RDX and HMX.Using cyanuric chloride and p-phenylenediamine as materials,potassium carbonatewas taken as neutralisatal reagents,THF as solvent,synthesized N,N′-di(4,6-di chlorine-1,3,5-s-triazine-2-base)-1,4-dipheylamine(comp.1),the yield may up to 90.0%,mp is319℃;synthesized azacalix[4]arenes (comp.3) by comp.1 and p-phenylenediamine (themole ratio 1:1),in room temperature, acetone as solvent ,the yield is 45.5%,mp>300℃.The product were characterized through IR and 1H NMR.Using cyanuric chloride and m-phenylenediamine as materials,potassium carbonatewas taken as neutralisatal reagents,THF as solvent,synthesized N,N′-di(4,6-di chlorine-1,3,5-s-triazine-2-base)-1,3dipheylamine (comp.2), the yield is 85.8%,mp is 300℃;synthesized azacalix[4]arenes (comp.4) by comp.2 and m-phenylenediamine (the moleratio 1:1),in room temperature,acetone as solvent,the yield is 30.0%, mp>300℃.Theproduct were characterized through IR and 1H NMR.Taking comp.3,comp.4 and sodium azide(the mole ratio 1:3) as materials,DMF assolvent.in 40~50℃, synthesized comp.5,comp.6, the yield is 90.0% , mp>300;In highpressure kettle, 80℃,dissolved comp.3,comp.4 to DMF,then connect ammonia t oDMF,get comp.7,comp.8. The product were characterized through IR and 1H NMR.The complex properties of aza-bridged calix[4]arene and RDX,HMX in solution wereinvestigated by fluorescence spectrum.The experiment results showed that when comp.5is added into the solution of RDX,it can get a steady compound.We also investigated thecomplex by XRD.The experiment results showed that there was reciprocity between hostand guest.