Preparation of p-nitrocalix[n]arene methyl ethers via ipso-nitration and crystal structure of tetramethoxytetra-p-nitrocalix[4]areneq
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چکیده
Nitration of p-tert-butylcalix[n]arene methyl ethers under a variety of reaction conditions has been examined. It has been determined that amongst different nitration procedures adopted (AlCl3/KNO3, HNO3/CH3COOH, HNO3/(CH3CO)2O, cerium(IV) ammonium nitrate/CH3COOH), ipso-nitration with CH3COOH/HNO3 gives best yields of p-nitrocalixarenes and work up conditions. ipso-Nitration of tetramethoxytetra-p-tert-butylcalix[4]arene gives tetramethoxytetra-p-nitrocalix[4]arene as triclinic crystals with space group M, with fl=9.102(3) A, £=11.623(3) A, c=18.368(3) A and a=77.99(2)8, j8=81.10(2)°, -y=73.37(2)°. Its conformation is partial cone and it forms an exocylic 1:1 complex with DMF.
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