flushed with nitrogen to remove traces of oxygen and water as
much as possible. All manipulations of both air- and moisturesensitive compounds were performed under a protective atmosphere (nitrogen or argon) using a glove box.
2.1 Synthesis
of VPCLF
1. Dichloromethane (DCM), anhydrous.
2. Trimethylaluminum in toluene.
3. 2-Hydroxyethyl vinyl ether (HEVE).
4. ε-CL (Aldrich). Further dried before use by 4 A ˚ molecular
sieves.
5. Isobutylaluminum bis(2,6-di-tert-butyl-4-methylphenoxide)
(IAB), composed of tris-isobutyl aluminum solution in hexane
and 2,6-di-tert-butyl-4-methylphenol.
6. Ground K 2 CO 3 . Dried overnight at 100
C in a vacuum oven.
7. Methanol.
8. Fumaryl chloride.
9. Reactor: a three-neck round-bottom glass flask with rubber
septum, a nitrogen/vacuum inlet, and thermometer.
10. Schlenk cones (25 mL and 250 mL).
11. Magnetic stirrer.
12. Buchner filtration device.
2.2 Stereolithography
1. N-Vinyl-pyrrolidone (NVP).
2. Lucirin TPO-L (ethyl-2,4,6-trimethylbenzoylphenylphosphinate) (BASF).
3. Orasol Orange G (Ciba Specialty Chemicals).
4. EnvisionTEC Perfactory Mini Multilens stereolithography
apparatus, equipped with a digital micro-mirror device which
enables projections of 1280x1024 pixels, each measuring
32 Â 32 μm
2 (see Note 1).
3 Methods
The synthesis of VPCLF should be run using Schlenk lines to
ensure a controlled atmosphere that includes any transfer of solvents and reagents to the polymerization reactor. The reactor and
other equipment used in the reaction (needles, Schlenk tubes, glass
syringes) should be kept overnight in an oven at 135
C to remove
traces of moisture and then quickly assembled and attached to a
Schlenk line.
3.1 Synthesis
of VPCL
1. Three cycles of vacuum and nitrogen have to be completed
before adding the reagents.
Stereolithography of VPCLF
57
much as possible. All manipulations of both air- and moisturesensitive compounds were performed under a protective atmosphere (nitrogen or argon) using a glove box.
2.1 Synthesis
of VPCLF
1. Dichloromethane (DCM), anhydrous.
2. Trimethylaluminum in toluene.
3. 2-Hydroxyethyl vinyl ether (HEVE).
4. ε-CL (Aldrich). Further dried before use by 4 A ˚ molecular
sieves.
5. Isobutylaluminum bis(2,6-di-tert-butyl-4-methylphenoxide)
(IAB), composed of tris-isobutyl aluminum solution in hexane
and 2,6-di-tert-butyl-4-methylphenol.
6. Ground K 2 CO 3 . Dried overnight at 100
C in a vacuum oven.
7. Methanol.
8. Fumaryl chloride.
9. Reactor: a three-neck round-bottom glass flask with rubber
septum, a nitrogen/vacuum inlet, and thermometer.
10. Schlenk cones (25 mL and 250 mL).
11. Magnetic stirrer.
12. Buchner filtration device.
2.2 Stereolithography
1. N-Vinyl-pyrrolidone (NVP).
2. Lucirin TPO-L (ethyl-2,4,6-trimethylbenzoylphenylphosphinate) (BASF).
3. Orasol Orange G (Ciba Specialty Chemicals).
4. EnvisionTEC Perfactory Mini Multilens stereolithography
apparatus, equipped with a digital micro-mirror device which
enables projections of 1280x1024 pixels, each measuring
32 Â 32 μm
2 (see Note 1).
3 Methods
The synthesis of VPCLF should be run using Schlenk lines to
ensure a controlled atmosphere that includes any transfer of solvents and reagents to the polymerization reactor. The reactor and
other equipment used in the reaction (needles, Schlenk tubes, glass
syringes) should be kept overnight in an oven at 135
C to remove
traces of moisture and then quickly assembled and attached to a
Schlenk line.
3.1 Synthesis
of VPCL
1. Three cycles of vacuum and nitrogen have to be completed
before adding the reagents.
Stereolithography of VPCLF
57