Specifications
4.
Check that the vessels are
fully
seated over the male Teflon
RV
fittings of the Lower
Drain Manifold. If the vesseIs are seated properly, the tops of the vessels will be
horizontally uniform and the frits will be seated just above or on the male Teflon RV
fittings of the Lower Drain Manifold
(Figure
10).
Figure
10.
Proper installation of the Quest RVs
11.
Coupling Reaction
To a bank of ten RV's (e.g., RVs
1-10,
Side A),
an
ArgoCap of PS-DES resin is added.
The capsule is dissolved by washing with DCM
(3
x
4
ml,
5
min. agitation). After
dissolving the ArgoCap, a solvent exchange with anhydrous NMP
(3
x 4
mL,
5
min.
agitation) is performed. Under nitrogen, the appropriate alcohol or carbonyl solution in
NMP
(0.3
M,
2
mL,
0.6
rnmol) is added to each RV
via
syringe. To this mixture,
Rl~cl(PPh~)~ solution in
NMP
(1
mL,
0.0075
M,
7.5
x
lo4
rnmol) is added under
nitrogen. The mixture is agitated for
3
h at
60°C
and then washed with NMP x 3, DCM x
3, and THF
x
2
(4 mL, agitate
5
min.). You may stop here if you do not wish to perform
the resin cleavage/scavenge. Instead of analyzing the cleaved products by GC,
qualitative IR analysis may be performed on the loaded resin. To prepare the resin for
analysis, dry the resin and take an IR spectra of the beads to see if the coupling reaction
was complete. Ether formation can be monitored by looking for the disappearance of the
Si-H IR stretch at
21 00
cm-'.
A.
Addition of PS-DES ArgoCaps to the RVs
1.
Drop one
150
mg
PS-DES ArgoCap into each
5
mL Teflon RV previously installed.
2.
Move the agitator to the
up
position by pushing the Agitation UP button located to the
right of the Quest Controller Unit display
(Figure
11).
Argonaut Technologies
Part
Number 102298
04/02/98
Quest Tutorial
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