Beruflich Dokumente
Kultur Dokumente
1789
1790
Table 1. Synthesis of PolyMA, PolyBA, PolyMMA, and PolySt by ARGET ATRP Using Ascorbic Acid as Reducing Agenta
monomer
ascorbic acid
(to Cu, in mol)
Cu (ppm)b
solvent
time (h)
conv (%)
Mn(theo)
Mn(GPC)
Mw/Mn
2c
3d
4d
MA
MA
MA
MA
10
10
10
10
250
250
25
25
DMF
anisole
DMF
anisole
5d
6e
7d
8d
9d
10f
MA
MA
BA
MMA
St
St
100
10
10
10
10
10
25
10
25
25
25
25
anisole
anisole
anisole
anisole
anisole
anisole
1.5
2.2
1.5
5.3
17
3.3
6
21.5
18
64.7
52
74
87
76
87
98
93
91
89
59
68
55
25 460
30 000
26 100
30 000
33 750
32 020
31 340
45 500
23 260
27 580
53 540
62 550
28 000
32 700
27 700
34 000
34 400
29 700
43 000
30 700
25 200
60 900
1.52
1.14
1.60
1.19
1.18
1.30
1.40
1.28
1.27
1.18
1.27
entry
1c
a Polymerizations were carried out in 60% solutions of monomer (in volume). Initiator: ethyl 2-bromoisobutyrate (EBiB) for MA, BA, and St; ethyl
R-bromophenylacetate for MMA. Ligand: Me6TREN. The amount of ligand has been fixed at 10 times the amount of Cu(II) initially added to the reaction
in order to ensure coordination of the ligand with Cu(II) in the presence of a large excess of monomer.27-29 Polymerization temperatures: 60 C for
MA, BA, and MMA; 90 C for St. b Concentration of Cu: molar ratio of Cu to monomer. c [M]:[I]:[Cu(II)] ) 400:1:0.1. d [M]:[I]:[Cu(II)] ) 400:1:0.01.
e [M]:[I]:[Cu(II)] ) 400:1:0.004. f [St]:[PMA-Br]:[Cu(II)] ) 400:1:0.01.
MA0702041