2-Mercaptoethanol → Acrylic acid vinylpyrrolidone

Participants

Reaction Steps

In a 500 mL three-necked flask, N-vinylpyrrolidone (33.34 g, 0.30 mol), acrylic acid (43.24 g, 0.60 mol), dimethyl sulfoxide (307.08 g), a polymerization initiator VA-061 (Wako Pure Chemical Industries, Ltd., 0.1408 g, 0.562 mmol) and 2-mercaptoethanol (43.8 μL, 0.63 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 20% 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 50° C. for 0.5 hours, followed by temperature rise to 70° C. and further stirring for 6.5 hours. After completion of the polymerization, the polymerization reaction solution was cooled to room temperature and 100 mL of water was added, and then the solution was poured into 500 mL of acetone and the mixed solution was left to stand overnight. On the next day, 200 mL of acetone was further added and then the supernatant was removed by decantation. The obtained solid component was washed seven times with acetone/water (=700 mL/100 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: 65 kD, Mw: 202 kD (Mw/Mn=3.1).

Provenance & Evidence