1. SINE 2020 – Chemical Deuteration WP FZJ Contributions
Jürgen Allgaier Jülich Centre for Neutron Science JCNS and Institute for Complex Systems ICS Forschungszentrum Jülich GmbH

2. Tasks Novel route for isoprene synthesis (D5.3, month 15)
Synthesis of deuterium labelled polythiophene based block copolymers (D5.5, month 20)
Synthesis of deuterium labelled polylactic acid (D5.8, month 30)
(Synthesis of L- and D-lactic acid, ESS deliverable D5.4)
(PEG/PEGylated lipids, D5.11)

3. Novel route for isoprene synthesis
accessibility/costs of starting compounds
monomer purity
deuteration degree

4. Synthesis of deuterium labelled polythiophene based block copolymers
1. GRIM Polymerization of P3HT

5. Synthesis of deuterium labelled polythiophene based block copolymers
2. Diblocks
P3HT: structural quality, chemical functionalization
impurities: homopolymers, salts
deuteration scenarios

6. Synthesis of deuterium labelled polylactic acid
lactic acid (h and d): ESS
lactide: FZJ
poly(lactic acid): RWTH (Prof. Okuda)

7. Synthesis of deuterium labelled polylactic acid
Lactide synthesis
D-lactic acid (h), 10g
52% LA, 48% open dimer
28% water LA
open dimer, 1H

8. Synthesis of deuterium labelled polylactic acid
Conversion to lactide
Purification by sublimation,
recrystallization: (yield: 2g, 35%)
lactide
open dimer, 1H
open dimer, 1H LA

9. THF; 18 h; ambient temperature
Synthesis of deuterium labelled polylactic acid
Polymerization (Dr. Beckerle, RWTH)
[ZnEt2]/[BnOH]/[L-Lactide]
1 / / Mn D
GPC (RI)
10 800
1.15
Corrected
6 300 -
Calculated
6 900
THF; 18 h; ambient temperature
96 % conversion (NMR)
13C{1H}NMR
iii
iis/
sii
isi

10. PEG
Polymerization of EO (h and d)
End group functionalization

11. PEG
Synthesis of maleimide functionalized PEGs