Methylation of partially O-benzylated p-tert-butylcalix[6]arenes follo
wed by hydrogenolysis constitutes an efficient method for the preparat
ion of partially O-alkylated calix[6]arenes in gram amounts, without a
dhering to column chromatography separations. Selective de-tert-butyla
tion followed by halogenation, or ipso-nitration of these precursors a
ffords calix[6]arenes containing bromo- or nitrosubstituents, respecti
vely, at precise positions of the upper rim.