2.3. Synthesis of Poly(N,N-(dimethylamino)ethyl methacrylate) Chain Transfer Agent (PDMAEMA-CTA)

YL Yiguo Li
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The PDMAEMA-CTA with a targeted polymerization degree of 160 were prepared as follows: DMAEMA (11.32 g, 0.072 mol), 2-cyano-2-propyl benzodithioate (CPDB) (0.10 g, 0.45 mmol) and azobisisobutyronitrile (AIBN) (0.01g, 0.06 mmol), were dissolved in 2 mL of toluene. The mixture was purged with nitrogen for 30 min and then heated at 60 °C for 24 h. The reaction was quenched by rapid cooling with ice-water. After the removal of toluene using a rotary evaporator, the mixture was dissolved in THF and precipitated in n-hexane. The polymer was filtered and dried under vacuum at room temperature overnight yield final product of 9.17 g (81 %). The molecular weight (Mn = 25,000 g·mol−1) and molecular weight distribution (PDI = 1.20) of the product were determined by SEC with PS standards. 1H NMR (400 MHz, CDCl3, δ): 0.86-1.10 (d, 370 H, CCH3 from PDMAEMA), 1.81 (270 H, CCH3CH2 from PDMAEMA), 2.22 (s, 820 H, N(CH3)2 from PDMAEMA), 2.50(t, 266 H, NCH2CH2O from PDMAEMA), 3.99(t, 266 H, NCH2CH2O from PDMAEMA), 7.79(m, 2H, o-ArH, from chain transfer agent), 7.46(m, 1H, p-ArH, from chain transfer agent). Polymerization degree of PDMAEMA was determined to be 133. Number-average molecular weight of PDMAEMA-CTA was determined to be 157 g·mol−1 × 133 + 221 g·mol−1 = 21,102 g·mol−1.

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