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Resin Selection

Default cycles are available for both standard resins (such as polystyrene) and high-swelling resins (such as PEG). It is 
important to use the appropriate cycles for the resin being used in the synthesis. When the resin type is selected in the   
Liberty Method Editor, the appropriate default cycles for that type will automatically be loaded.
Although most resins are compatible with microwave SPPS on the Liberty Blue, CEM recommends the resins shown in the 
table below for optimal results.

Peptide Length

C-Terminal Acid

C-Terminal Amide

Standard (<25 residues)

Cl-TCP(Cl) ProTide

TM

Fmoc Rink Amide ProTide

TM

Long (>25 residues)

Cl-MPA ProTide

TM

 (LL)

Fmoc Rink Amide ProTide

TM

 (LL)

Mesh Size 

Only 100-200 mesh (or lower) resin (>75 micron) should be used with the Liberty Blue. The use of higher mesh resins will 
result in clogging of the reaction vessel frit and damage to the system.

Special Case: Hyper Acid Sensitive Resins (e.g. 2-chlorotrityl)

Acidic additives (HOBt, HOAt, Oxyma) can lead to premature cleavage of the peptide from the resin (low yields). Activation 
methods containing DIEA are more basic and thus preferred to DIC/Oxyma for these resins at high temperatures. Since 
lower temperatures should be used, the more aggressive HATU activator is recommended.

CEM Corporation offers Cl-TCP(Cl) ProTide which shows excellent stability to high temperatures and acidic additives such 
as Oxyma Pure, yet still exhibits hyper-acid sensitivity.  The Cl-TCP(Cl) ProTide resin can be cleaved under 1% TFA/DCM 
conditions.

CEM Preference Reagents

Resin/Linker

Coupling Microwave Method

1

Exceptions

1

AA/DIC/Oxyma

2

 in DMF

Cl-TCP(Cl) ProTide Resin

Standard Coupling (90°C 2 min)

N/A

3

2-Chlorotrityl resin

60°C 5 min Coupling

4

N/A

3

2

AA/HBTU/DIEA

5

 in DMF

Cl-TCP(Cl) ProTide Resin

75°C 5 min Coupling

Cys/His: 50°C 10 min Coupling

2-Chlorotrityl resin

50°C 10 min Coupling

N/A

1

Standard deprotection (90

°

C 1 min) can be performed in all cases.

2

0.1 equivalents DIEA should be added to Oxyma solution

3

Recommended Coupling Microwave Method assumes employment of His(Boc).  For other His derivatives, use 50

°

C 10 min Coupling Micro-

wave Method.

4

Coupling time can be extended to 10 min.

5

DIEA should be prepared in NMP.

Содержание liberty

Страница 1: ...e is designed to highlight the basic chemistry and functions of the Liberty Blue Read and understand the Manual PN 600291 before operating the Liberty Blue For More Information Liberty Blue Operation Manual PN 600291 detailed information about setup and operation of the system CEM website www cem com list of spare parts pictures latest information about CEM s products references application notes ...

Страница 2: ... 5 0 mmol Wash Solvent DMF DMF DMF DMF DMF DMF Deprotection Cocktail 4 Piperidine in DMF or 2 Piperazine w v in EtOH NMP 10 90 4 Piperidine in DMF or 2 Piperazine w v in EtOH NMP 10 90 20 Piperidine in DMF or 10 Piperazine w v in EtOH NMP 10 90 20 Piperidine in DMF or 10 Piperazine w v in EtOH NMP 10 90 20 Piperidine in DMF or 10 Piperazine w v in EtOH NMP 10 90 20 Piperidine in DMF or 10 Piperazi...

Страница 3: ...re cleavage of the peptide from the resin low yields Activation methods containing DIEA are more basic and thus preferred to DIC Oxyma for these resins at high temperatures Since lower temperatures should be used the more aggressive HATU activator is recommended CEM Corporation offers Cl TCP Cl ProTide which shows excellent stability to high temperatures and acidic additives such as Oxyma Pure yet...

Страница 4: ...istidine His Boc suppresses epimerization at elevated temperature and by default is coupled using the standard coupling microwave method His Trt is susceptible to epimerization at elevated temperature His Trt should be coupled using the single 50 C 10 min couplpling cycle to minimize epimerization using the parameters in the table below Stage Temp o C Power W Time sec Delta T 1 25 0 120 2 2 50 35 ...

Страница 5: ...eavage of the peptide In these cases the use of Fmoc Asp OMpe OH in place of the more common Asp OtBu can reduce aspartimide formation without the addition of Oxyma Pure HOBt The Asp Gly DG segment is particularly sensitive to base catalyzed aspartimide formation Simple addition of HOBt or Oxyma Pure to the standard deprotection solutions may not be sufficient to prevent this side reaction The use...

Страница 6: ...sses oxidation of Cys Met side chains Cleavage can be performed either at room or elevated temperatures The table below lists CEM s recommended parameters for both elevated and room temperature cleavage For sequences with more than 3 arginine residues extend cleaving time by 5 minutes per Arg after 3 if using heated cleavage or by 30 minutes if using room temperature cleavage Avoid cleaving for ov...

Страница 7: ...positions Reaction Scale for Resin Transfer The resin transfer option is intended for syntheses at 0 1 or 0 25 mmol scale 0 25 1 0 g of resin The resin transfer option should only be used with the 30 mL reaction vessel This option has not been optimized by CEM for use with the 125 mL vessel Transfer Solvent The transfer solvent is used to move the resin into and out of the reaction vessel and to s...

Страница 8: ...ty coated glass 250 mL Bottle used for Activator Base 551325 500 mL Bottle Safety coated glass 500 mL Bottle used for Deprotection 551330 1 L Bottle Safety coated glass 1 L Bottle used for wash solvent 177285 6 L Carboy Plastic 6 L carboy used for waste Temperature Probe Part Number Name Description 314325 Fiber Optic Probe Probe used to measure and control reaction temperature Reaction Vessel Sel...

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