N,N-Diethylacrylamide → N,N-diethyl acrylamide N,N-dimethylacrylamide

Participants

Reaction Steps

In a 300 mL three-necked flask, N,N-diethyl acrylamide (DEAA, 19.22 g, 0.151 mol), N,N-dimethylacrylamide (DMA, 14.88 g, 0.150 mol), TAA (104.65 g) and a polymerization initiator VA-061 (Wako Pure Chemical Industries, Ltd., 0.0465 g, 0.186 mmol) were charged, and then equipped with a three-way stop-cock, a reflux condenser tube, a thermometer and a mechanical stirrer. The concentration of the monomer was 25% by weight. After degassing inside the three-necked flask using a vacuum pump and repeating replacement by argon three times, stirring was carried out at 70° C. for 1.5 hours, followed by temperature rise to 75° C. and further stirring for 3.5 hours. After completion of the polymerization, the polymerization reaction solution was cooled to room temperature and the solvent was distilled off by an evaporator, and then washed once with each of n-hexane/methanol (=500 mL/0 mL, 250 mL/25 mL, 200 mL/30 mL and 200 mL/3 mL). The solid component was dried overnight by a vacuum drying oven at 60° C. Liquid nitrogen was charged and the solid component was crushed by a spatula, and then dried by a vacuum drying oven at 60° C. for 3 hours. The thus obtained copolymer had a molecular weight of Mn: 90 kD, Mw: 327 kD (Mw/Mn=3.7).

Provenance & Evidence