1 Supporting Information Novel Alkoxyamines for the Successful Controlled Polymerization of Styrene and Methacrylates Alexandre Simula, 1 Miren Aguirre, 1 Nicholas Ballard, 1 Antonio Veloso, 1 José R. Leiza, 1 Steven van Es 1,2 and José M. Asua 1, * 1 POLYMAT and Kimika Aplikatua Saila, University of the Basque Country UPV/EHU, Joxe Mari Korta Zentroa, Tolosa Hiribidea 72, 20018, Donostia/San Sebastián, Spain 2 Dispoltec BV, PO Box 331, 6160 AH Geleen, The Netherlands Conversion Determination for Polymerization of Styrene in the Presence of Alkoxyamine Equation (1)  =   +   +     +   ×    ‒      ‒   Polymerization of Styrene in the Presence of Alkoxyamine (B) In a typical procedure, Alkoxyamine (B) (857 mg, 2.52 mmol), styrene (87.6 g, 333 equiv, 75 wt.%) and tert-butylbenzene (29.5 g) were charged into a three-neck 250-mL RBF fitted with a stirring bar, thermometer and rubber seals. The mixture was stirred and deoxygenated with nitrogen for 30 minutes and subsequently placed in a pre-heated oil bath at 136 °C. The solution was left to polymerize at 126 °C for at least 5 hours. Samples for conversion and SEC analysis were carefully taken from the polymerization mixture via a deoxygenated syringe. Monomer conversion was calculated from gravimetric analysis using Equation 1. After polymerization, the solution was diluted in THF, precipitated in MeOH and dried under vacuum to yield a white solid. Electronic Supplementary Material (ESI) for Polymer Chemistry. This journal is © The Royal Society of Chemistry 2017