Dirhodium (I1) caprolactamate, Rhz (capI4, catalyzes diazo decomposition of cycloalkylmethyl diazoacetates which form spirolactones in moderate to high yield by insertion into a tertiary carbonhydrogen bond. Similar results are obtained with diazoacetates derived from tetrahydropyran-2-methanol and tetrahydrofurfuryl alcohol but not from cyclopropylmethanol. With tetrahydrofuran-3-ylmethyl diazoacetate, Rhz (cap) 4 ...