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. 2022 Sep 20;13(39):11540–11550. doi: 10.1039/d2sc04210j

EY/Cu dual catalysis: optimization of ATRP conditionsa.

No. EYH2 (equiv) CuBr2 (equiv) TPMA (equiv) rpmb Conv.c (%) M n,th M n,abs d M n,app e Đ e
1 0.2 0.6 0 0
2 0.05 0.6 0 89 89 000 187 500 126 000 4.30
3 0.05 0.2 0.6 0 88 88 000 84 000 65 000 1.19
4 0.05 0.2 0.6 250 86 86 000 82 500 64 000 1.18
5 0.05 0.2 0.6 500 86 86 000 86 000 66 000 1.15
6 0.05 0.2 0.6 1000 86 86 000 86 000 66 000 1.18
7 0.1 0.2 0.6 500 89 89 000 89 500 68 500 1.20
8 0.01 0.2 0.6 500 84 84 000 79 500 62 000 1.15
9 0.005 0.2 0.6 500 80 80 000 73 000 58 000 1.16
10 0.01 0.3 0.6 500 74 74 000 70 000 56 000 1.14
11 0.01 0.1 0.6 500 92 92 000 90 500 69 000 1.21
12 0.01 0.2 0.4 500 77 77 000 61 000 50 000 1.19
13 0.01 0.2 1.2 500 91 91 000 90 500 69 000 1.16
a

Reactions conditions: [OEOMA500]/[HOBiB]/[EYH2]/[CuBr2]/[TPMA] = 200/1/x/x/x, [OEOMA500] = 300 mM, in PBS with DMSO (10% v/v), irradiated for 30 min under green LEDs (520 nm, 9.0 mW cm−2) in an open vial with stirring at 0–1000 rpm.

b

Revolutions per minute (rpm).

c

Monomer conversion was determined by using 1H NMR spectroscopy.

d

Molecular weight (Mn,abs) was determined by Mark–Houwink calibration.

e

Apparent molecular weight (Mn,app) and dispersity (Đ) were determined by GPC analysis (DMF as eluent) calibrated to poly(methyl methacrylate) standards.