LCrK (Cat. 2) catalysed PTA ROCOP with 3-Me/3-R-substituted oxetanesa.
Runb | R | t [h] | Conv.a [%] | Alt.c [%] | M n d [kDa] (Ð) |
---|---|---|---|---|---|
#1 | Me | 19 | 99 | 99 | 11.4 (1.2) |
#2 | CH2OEt | 60 | 75 | 99 | 28.4 (2.2) |
#3* | CH2OBn | 72 | 80 | 97 | 9.8 (1.2) |
#4 | CH2OAllyl | 220 | 60 | 99 | 16.2 (1.6) |
ROCOP conducted at 80 °C or *120 °C with 1 eq. LCrK: 1000 eq. 3-Me,3′-R-Oxetane: 1000 eq. PTA.
Conversion calculated by comparing the relative integrals in the normalised 1H NMR spectrum (CDCl3, 400 MHz) of aromatic resonances due to polymer versus unconsumed PTA.
Relative integrals in the 13C NMR spectrum (CDCl3, 126 MHz) from carbonyl resonances due to alternating ester-alt-thioester links compared to other carbonyl resonances.
Determined by GPC (gel permeation chromatography) measurements conducted in THF, using narrow MW polystyrene standards to calibrate the instrument.