|Although the chemistry of corroles has grown spectacularly in recent years, the field has been marred by the lack of convenient protocols for demetalation of metallocorroles. In this thesis, I have developed a superior procedure for demetalating copper corroles with concentrated
H2SO4 and 5-200 equiv FeCl2 or SnCl2. The yields obtained with this reductive procedure are
generally substantially better than with HCl3/H2SO4, CH2Cl2/H2SO4, or H2SO4 alone. With an
oxidation-prone metallocorrole such as Cu[T(p-OMeP)C], the reductive protocol was essential
for obtaining any measurable yield of the free base at all. Free-base β-octabromo-mesotriarylcorroles were also obtained in pure form, in good yields, and with relative ease via this procedure.