Abstract The Michael addition of dimethyl malonate (12) to tert-butyl acrylate (11), carried out without solvent, affords the triester 13a in 88% yield on a kg scale. Selective partial hydrolysis of 13a produces the monoacid 13b almost quantitatively. The Kolbe electrolysis of 13b furnishes the tetraester 7c as a crystalline 1: 1 mixture of diastereomers in 62–74% yield. The Dieckmann condensation of 7c is induced by sodium hydride/tert-butyl alcohol ...