111.
CleavageIScavenger of the Resin and Product Collection
Cleavage solution (0.4
M
HFIPyridine in THF,
4
mL) is added to the washed resin using
a syringe and the mixture agitated for
2
h at room temperature. HF scavenger
(Me;SiOMe,
0.5
mL) is added to each RVs
via
syringe and the mixture agitated at room
temperature for an additional
2
h. The solvent from each RV is collected into
10-preweighed scintillation vials. The resin is then washed twice with THF
(3
mL,
5
min. agitation). The wash solvent is collected into the 10 scintillation vials used above.
The solvent is evaporated from the samples using a Savant SpeedVac (SpeedVac, 60 min,
no heating) and the products weighed to determine the mass yield. THF
(1
ml)
is added
to each scintillation vial and the solutions analyzed by GC for product purity.
Addition of Cleavage Solution to the
RVs
Provide a low flow rate nitrogen sweep of the RVs during the addition of cleavage
solution (HFIPyridine in
THF)
by turning the Manifold Control Valves to
"UTILITY
1"
and "METERED GAS". Gas will flow out of the Utility
1
port to
the oil bubbler.
Adjust the Metered Gas Needle Valve located on the top of the Quest Reactor
Unit until you see a steady stream of gas bubbling through the oil bubbler when
one of the Luer Plugs is removed from the Upper Manifold. This will ensure the
establishment of an inert atmosphere during the addition of solvent or reagent
through the Upper Manifold Addition Port. Modify the gas flow by turning the
Metered Gas Needle Valve counter clockwise (left) to increase the gas flow rate
and clockwise (right) to decrease the gas flow rate.
Remove the Luer Plug from the first RV Luer Port (twist and pull) and insert the
syringe needle below the Teflon lines of the male Teflon RV fitting (below the
stream of
Nz).
Dispense
4
mL of HFIPyridine solution in THF. Take care not to
score the interior surfaces of the Luer Port with the needle, as marring the surface
can affect the sealing of the Luer Port. After delivery, replace the Luer Plug
(twist and push) and add cleavage solution to the remaining
9
RVs.
During the cleavage, keep the RVs under a nitrogen blanket by first turning the
Manifold Control Valves to "CLOSED" and "METERED GAS" and then turning
both of the Manifold Control Valves to "CLOSED".
Adjust the Agitation
Bar
by doing the following:
Raise the Agitation
Bar
up by pushing the Agitation UP soft key located to the
right
of
the Quest Controller Unit display.
Use the
7/64"
hex wrench supplied with the Quest to loosen the Agitation Stops.
Adjust the Agitation Stops on the Reactor Unit so the maximum magnet height is
-2
cm below the solvent level in the RVs. Tighten the Agitation Stops so both
stops are at the same height.
On the Quest Controller Unit press the MODE soft key located below the
LCD
display until the Agitation menu is displayed. Set the agitation parameters as
follows: Mix Every 4.0sec. and %Upward=
60°h.
Argonaut Technologies
Part Number 102298
04/02/98
Quest Tutorial
Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com
(33 pages)
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