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. 2024 Feb 21;12(12):4933–4945. doi: 10.1021/acssuschemeng.3c07993

Table 3. Polymerization of nBA and tBA in Cygnet 0.0 via SARA ATRPa.

entry monomer [Cu/L]0 [ppm] t [h] convb [%] kpappb Mn,theoc Mn,appd Mw/Mnd Ieffe [%]
1 nBA 300 1.50 82 1.074 8,580 7,290 1.18 118
2 tBA 300 1.75 99 2.419 10,310 8,950 1.21 115
3 nBA 100 2.50 91 0.621 9,550 8,010 1.14 119
4 nBA 75 22.5 88 0.095 9,200 7,600 1.12 121
5 nBA 50 8.25 no conversion
a

General reaction conditions: T = 75 °C; Vtot = 4 mL; argon atmosphere; [monomer]0 = 50% v/v; [nBA]0 = 3.45 M for entries 1, 3–5, [tBA]0 = 3.38 M for entry 2, [monomer]0/[EBiB]0/[CuIIBr2/Me6TREN]0 = 80/1/0.024 for entries 1 and 2, [nBA]0/[EBiB]0/[CuIIBr2/Me6TREN]0 = 80/1/0.008 for entry 3, [nBA]0/[EBiB]0/ [CuIIBr2/Me6TREN]0 = 80/1/0.006 for entry 4, [nBA]0/[EBiB]0/ [CuIIBr2/Me6TREN]0 = 80/1/0.004 for entry 5. SARA ATRP with copper wire: d = 0.1 cm, l = 4 cm.

b

Monomer conversion, apparent rate constant of propagation (kpapp), and apparent theoretical degree of polymerization of monomer unit (DPn,theo) were determined by NMR.

c

Mn,theo = ([monomer]0/[EBiB]0) × conversion × MMonomer + MEBiB.

d

Apparent Mn and Mw/Mn were determined by GPC.

e

Initiation efficiency, Ieff = (Mn,theo/Mn,app) × 100%.