“…The preparation of cone ‐7,15,23‐triethoxycarbonyl‐25,26,27‐tris( N,N ‐diethylaminocarbonylmethoxy)‐2,4,10,12,18,20‐hexahomo‐3,11,19‐trioxacalix[3]arene ( cone ‐ 4 ) is shown in Scheme . Thus, bis(hydroxymethylation) of ethyl‐4‐hydroxybenzoate ( 1 ) with formaldehyde in aqueous NaOH for one week afforded ethyl‐3,5‐bis(hydroxymethyl)‐4‐hydroxybenzoate ( 2 )15 in 41 % yield. Heating compound 2 to reflux in p ‐xylene for 24 hours afforded hexahomotrioxacalix[3]arene 3 11a.…”