38
Setting up a Synthesis
NOTE
All reagent positions must have a centrifuge tube in place. If a given reagent is not required for a
synthesis, connect an empty centrifuge tube to that position.
2. Connect activator base and activator bottles to the appropriate positions on the system.
NOTE
It is important that the reaction vessel be empty before running the Change Bottle Deprotection operation.
The Change Bottle Deprotection operation will add deprotection solution to the reaction vessel as part of
the priming procedure, and then wash the reaction vessel with main solvent.
3. Check the level of deprotection solution remaining in the deprotection bottle. If more deprotection is required,
use the Change Bottle Deprotection operation to replace the bottle (see Change Bottle Deprotection in Section
4).
3.1. From the Options menu, select Maintenance.
3.2. From the Change Bottle folder, select the Change Bottle Deprotection operation and click Run
Operation.
3.3. The Change Bottle window will appear. Follow the on screen instructions to depressurize and remove
the existing bottle.
3.4. Add the required volume of deprotection solution to the bottle. Ensure the reagent line has a main
solvent lter in place (PN 551000), then connect the bottle to the cap.
3.5. Click OK to continue with the Change Bottle procedure. The Liberty Blue will automatically pressurize
the bottle and click OK to prime the lines.
4. Check the level of solvent remaining in the solvent bottle. If more solvent is required, use the Change Bottle Main
Solvent operation to replace the bottle. (see Change Bottle Main Solvent).
4.1. From the Options menu, select Maintenance.
4.2. From the Change Bottle folder, select the Change Bottle Main Solvent operation and click Run
Operation.
4.3. The Change Bottle window will appear. Follow the on screen instructions to depressurize and remove
the existing bottle.
4.4. Ensure the dip tube has a main solvent lter (PN 551000) in place, then screw the cap onto the
solvent bottle.
4.5. Click Next to continue with the Change Bottle procedure. The Liberty Blue will automatically pressurize
the bottle and prime the lines.
5. Add the resin to the reaction vessel.
WARNING
It is vital to use the appropriate reaction vessel for the scale of the synthesis. The standard (30 mL)
vessel should be used for syntheses between 0.005 and 0.25 mmol scale (up to 1 g of resin maximum).
The large (125 mL) vessel should be used for syntheses at 0.5 mmol scale and higher (up to 8 g of resin
maximum).
To replace the vessel:
1. Remove the reaction vessel from the microwave cavity.
2. Disconnect the bottom tting of the brown union connector.
3. Disconnect the vessel body from the attenuator.
4. Disconnect the ltered drain line from the vessel body at the brown tting.
5. Connect the bottom portion of the union to the new vessel body.
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