无溶剂法合成杯[4]芳烯星形化合物

The p-phenylenedialdehyde mono-acetal was prepared by the reaction of p-phenylenedialdehyde with acetic anhydride in the presence of InBr3. The calyx[4]resorcinarene was prepared using the p-phenylenedialdehyde mono-acetal and resorcinol as starting materials. By pestling pentaerythritol and calyx[4]resorcinarene, and then pestling the intermediate and 3-4-(dioxolan-2'-yl)phenyl-9-(4-diacetoxy-methyl)phenyl-2,4,8,10-tetraoxaspiro[5.5]undecane, the calyx[4]resorcinarenes star compound was synthe-sized under a solvent-free condition. After the pestling, the mixture was washed with water and recrystallised from the mixture of ethanol and acetone (V:V=1:1). The product and intermediates were characterized by IR, 1H NMR, MS spectra and elemental analysis.