The dimethylphosphono-substituted diazoalkanes PhC (Nz) P (0)(OMe) z and N2CHP (0)(OMe) 2 have been prepared, the first via the tosylhydrazone route, and the second by diazotization of the amine, and both could be isolated as the pure compounds. Their copper- catalyzed decomposition in the presence of olefins serves well in the preparation of dimethylphosphono-substituted cyclopropanes. Dimethyl cy-diazobenzylphosphonate ...