SILICYCLE MiniBlock Manuel utilisateur

www.SiliCycle.com

SiliCycle MiniBlock®

User Guide

SiliCycle MiniBlock® User Guide

2www.SiliCycle.com | inf[email protected]om

1. Usage and Safety Precauons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

Cleaning .................................................................................................... 6

Maintenance ............................................................................................... 6

Storage ..................................................................................................... 6

Temperature ................................................................................................ 6

Pressure .................................................................................................... 6

Components ................................................................................................ 6

Document Convenons ...................................................................................... 6

2. General .................................................................................... 7

2.1. The SiliCycle MiniBlock Reacon Tubes .................................................................... 8

2.2. SiliCycle MiniBlock Conguraons ....................................................................... 10

2.2.1. Ambient Temperature Conguraons ............................................... 11

2.2.2. Plugs for Unused Pinch-Tube Inserts ................................................ 11

2.2.3. Controlled Temperature Conguraons ............................................. 11

2.2.4. Combining Red and Blue SiliCycle MiniBlocks Into 96-Well Format ....................... 12

2.3. SiliCycleMiniBlock System Materials .................................................................... 12

2.3.1. SiliCycle MiniBlock Metal Components .............................................. 12

2.3.2. Reacon Tube Materials .......................................................... 12

2.3.3. Pinch-Tube Insert Materials ....................................................... 12

2.3.4. Septa Materials ................................................................. 13

2.4. SiliCycleMiniBlock Temperature Control ................................................................. 14

2.5. SiliCycle MiniBlock Reacons Requiring an Inert Atmosphere .............................................. 15

3. SiliCycle MiniBlock Assembly and Reacon Setup ................................................ 16

3.1. Pre-Assembly Checks .................................................................................. 16

3.2. SiliCycle MiniBlock Assembly ........................................................................... 18

3.2.1. Setup for Ambient Temperature Reacon ............................................ 18

3.2.2. Setup for Controlled Temperature Reacon .......................................... 18

3.2.3. Inserng Reacon Tubes .......................................................... 19

3.2.4. Sealing for Reacons Not Requiring Inert Condions .................................. 20

3.2.5. Sealing for Reacons Requiring Inert Condions ...................................... 22

3.2.6. Closing the SiliCycle MiniBlock Valve ................................................ 23

4. Reacon Setup, Mixing and Incubaon ......................................................... 24

4.1. Resin Addion – Solid-Phase Reacons .................................................................. 24

4.1.1. Resin Addion – Serial ........................................................... 24

4.1.2. Resin Addion – Parallel .......................................................... 24

4.1.3. IRORI® Kans™ ................................................................... 24

4.1.4. Resin Swelling .................................................................. 24

4.2. Inert Atmosphere ..................................................................................... 24

4.3. Adding Solvents and Reagents .......................................................................... 25

4.4. Reacon Mixing and Incubaon ........................................................................ 26

4.4.1. Shaking Staons ................................................................ 26

4.4.1.1. Securing SiliCycle MiniBlocks on the Shaking Staon ................................. 26

4.4.1.2. Balancing the Shaking Staon .................................................... 26

4.4.1.3. Pre-Operaonal Shaking Staon Check ............................................ 27

4.4.1.4. Seng Agitaon Speed ......................................................... 28

4.5. Incubaon ............................................................................................ 28

4.5.1. Aaching the Manifold to the Shaker ............................................... 28

4.5.2. Connecng to the Recirculator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

4.5.3. Tesng the Recirculaon System ................................................... 29

5. Washing, Puricaon and Product Collecon .................................................... 30

5.1. Solvent Removal and Resin Washing .................................................................... 30

5.1.1. Removing Solvents to Waste on the Shaking Staon ................................... 30

5.1.2. Accelerang Solvent Drainage ..................................................... 30

5.1.2.1. Air Push Assist Device .......................................................... 31

5.1.2.2. Posive Pressure Manifold ...................................................... 31

5.1.2.3. Inert Atmosphere Manifold ...................................................... 32

5.1.3. Washing ....................................................................... 32

5.2. Puricaon and Clean-Up .............................................................................. 32

5.2.1. Solid-Phase Extracon ( SPE)....................................................... 32

5.2.2. Scavenger Resins ................................................................ 33

5.3. Product Collecon / Cleavage ........................................................................... 33

5.3.1. Collecon Rack Selecon ......................................................... 34

5.3.2. Collecon Vessel Posioning ...................................................... 37

6. Maintenance .............................................................................. 39

6.1. Cleaning Procedure .................................................................................... 39

6.1.1. Post-Collecon Rinse ............................................................. 39

6.1.2. SiliCycle MiniBlock Cleaning ....................................................... 40

6.2. Replacing Consumable Components .................................................................... 40

6.2.1. Replacement of Pinch-Tube Inserts ................................................. 40

6.2.2. Replacement of Compression Cords ................................................ 42

7. Troubleshoong ............................................................................ 43

7.1. Jammed Slide Valve ................................................................................... 43

7.2. Leakage / Solvent Loss ................................................................................. 43

7.3. Prevenve Maintenance ............................................................................... 45

Appendix A: Heat Shrinking Teon® Sleeves Onto Glass Reacon Tubes ................................ 48

A.1. Apparatus ............................................................................................ 48

A.2. Procedure ............................................................................................ 48

A.3. Quality Checks ........................................................................................ 49

A.3.1. Incomplete Heat-Shrinking ........................................................ 49

A.3.2. Defecve Heat-Shrinking ......................................................... 49

Appendix B: Resin Dispenser: Operang Instrucons ............................................... 50

B.1. Overview ............................................................................................. 50

B.2. Operaon Descripon ................................................................................. 50

B.3. Dispensing............................................................................................ 51

B.3.1. Resin Dispenser Setup ( Procedure wrien for the 48-Posions Version )................... 51

B.3.2. Dispensing Procedure ............................................................ 52

B.3.3. Dispensing to Microter / Deep Well Plates .......................................... 53

B.4. Resin Cleaning ........................................................................................ 54

B.5. Resin Dispenser Calibraon ............................................................................ 54

Appendix C: SiliCycle MiniBlock Collecon Rack Conguraons ....................................... 55

C.1. Assembly Diagrams .................................................................................... 56

Appendix D: Determining Correct Collecon Tube Height ............................................ 58

D.1. Instrucons for the Go/No-Go Test ...................................................................... 58

Appendix E: Chemistry Applicaons .............................................................. 59

Procurement ................................................................................ 59

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Figures

Figure 1: SiliCycle MiniBlock ..................................................................... 7

Figure 2: Reacon Tube Components ............................................................. 8

Figure 3: SiliCycle MiniBlock Components .......................................................... 8

Figure 4: Glass Reacon TubeWith Teon® Heat Shrink Sleeve ......................................... 8

Figure 5: Types of Pinch-Tube Inserts .............................................................. 9

Figure 6: Valve Mechanism in Closed Posion ...................................................... 9

Figure 7: SiliCycle MiniBlock with Valve Key ........................................................ 9

Figure 8: Reacon Tube Conguraons ........................................................... 10

Figure 9: Red Plugs Conguraons ............................................................... 11

Figure 10: SiliCycle MiniBlock Heat Transfer Blocks ................................................. 11

Figure 11: Collecon conguraon 96-Posions .................................................... 12

Figure 12: SiliCycle MiniBlock with Heat Transfer Block .............................................. 14

Figure 13: Inert/Purge Manifold ................................................................. 15

Figure 14: Slide Valve Operaon ................................................................. 16

Figure 15: Inspecng Pinch-Tubes ............................................................... 17

Figure 16: Pinch-Tube Extension . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

Figure 17: AlignmentsPlates Installed ............................................................ 18

Figure 18: Heat Transfer Block Installed ........................................................... 19

Figure 19: Insert Reacon Tubes ................................................................ 19

Figure 20: Male / Female Luer Fing ............................................................ 20

Figure 21: Seang Reacon Vessels .............................................................. 20

Figure 22: Septum Layer and Cover Plate ......................................................... 21

Figure 23: Inert / Purge Manifold ................................................................ 22

Figure 24: SiliCycle MiniBlock With Valve Key ...................................................... 23

Figure 25: Dispensing Plate ..................................................................... 24

Figure 26: Shaking Staons ..................................................................... 26

Figure 27: Aligning SiliCycle MiniBlocks on the Shaker Top ( With Oponal Recirculator Manifold )........... 27

Figure 28: Securing SiliCycle MiniBlocks on the Shaker Top ........................................... 27

Figure 29: Aaching the Recirculator Manifold to the Shaker Top ..................................... 28

Figure 30: Slide Valve Operaon ................................................................. 30

Figure 31: Air Push Assist Device ................................................................ 31

Figure 32: Posive Pressure Manifold ............................................................ 31

Figure 33: Transfer to Second SiliCycle MiniBlock Containing SPE Packed Tubes ( Using Transfer Adapter ).....32

Figure 34: Examples of SiliCycle MiniBlock Collecon Racks and Plates ................................. 33

Figure 35: Collecng Products .................................................................. 34

Figure 36: Vacuum Collecon Base, Shown With a 24-Posions Rack .................................. 34

Figure 37: Proper Height Alignment for Collecon Tubes ............................................ 37

Figure 38: Posioning SiliCycle MiniBlock Components For Collecng Into 48 Test Tubes Rack .............. 38

Figure 39: Pinch-Tube Extension . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

Figure 40: Tube Removal Tool ................................................................... 39

Figure 41: Remove Valve Insert Lock-Plate ........................................................ 41

Figure 42: Remove Pinch Tube Inserts ............................................................ 41

Figure 43: Compression Cords Replacement ....................................................... 42

Figure 44: Leakage Points ...................................................................... 43

Figure 45: Exploded View of SiliCycle MiniBlock Reactor ............................................. 46

Figure 46: Glass Reacon Tube with Teon® Sleeve ................................................. 48

Figure 47: Resin Dispensing Plate ................................................................ 50

Figure 48: Resin Dispenser ( 13742086)........................................................... 51

Figure 49: Resin Dispenser Closed Posion ........................................................ 52

Figure 50: Resin Dispensing Spreader ............................................................ 52

Figure 51: Dispensing Powder .................................................................. 53

Figure 52: Replacing the Plate .................................................................. 54

Figure 53: The Vacuum Collecon Base Set ( 13742008)............................................. 55

Figure 54 : 12 x 100 mm Test Tubes ( 8 mL)........................................................ 56

Figure 55 : 12 x 75 mm Test Tubes ( 6 mL)......................................................... 56

Figure 56 : Deep Well Plate ( Various Volumes )..................................................... 56

Figure 57 : Tall Minitube Rack ( 2.5 mL)........................................................... 56

Figure 58 : 16 x 100 mm Test Tubes ( 15 mL)....................................................... 57

Figure 59 : 15 x 45 mm Vials (3.7 mL)............................................................. 57

Figure 60: 17 x 61 mm Vials (7.5 mL) ............................................................ 57

Figure 61 : 21 x 70 mm Vials (15 mL)............................................................. 57

Figure 62 : 28 x 95 mm Vials ( 40 mL)............................................................. 57

Figure 63: Tube Heights are Correct. “GO” ........................................................ 58

Figure 64: Tube Heights are too Low. “NO-GO” .................................................... 58

Figure 65: Tube Heights are too High. “NO-GO” .................................................... 58

Tables

Table 1: MinBlock Physical Descripon ............................................................ 7

Table 2: SiliCycle MiniBlock Conguraons ........................................................ 10

Table 3: SPE Development Kits Available from SiliCycle .............................................. 33

Table 4: Collecon Plates, Racks and Vessels ...................................................... 36

Table 5: SiliCycle MiniBlock Spare Parts .......................................................... 47

Table 6: Standard Conguraons ................................................................ 51

Table 7: High Volume Kit ( Sold Separately )........................................................ 51

Table 8: Collecon Rack Conguraons ........................................................... 55

SiliCycle MiniBlock® User Guide

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1. Usage and Safety Precauons

The SiliCycle MiniBlock products for parallel synthesis are intended for use by persons skilled in chemical handling and synthesis. Best results with

the SiliCycle MiniBlock can be achieved by following the usage, maintenance and storage guidelines in this Operaons Manual.

SiliCycle MiniBlock products include a 12 month warranty. This warranty is conngent on proper usage and maintenance as described in this

manual. If instrucons contained in this manual are not followed, the warranty may be invalidated. Some of the common consideraons for opmal

SiliCycle MiniBlock use include:

Cleaning

All chemicals should be cleaned from the SiliCycle MiniBlock as soon as possible. Full cleaning of the SiliCycle MiniBlock is recommended

immediately aer synthesis.

Maintenance

SiliCycle MiniBlocks should be checked and consumable components replaced as part of a scheduled maintenance program.

Storage

SiliCycle MiniBlocks should be stored with the slide (drainage) valve in the open posion and the two side clamps le undone.

Temperature

Reacon temperatures are limited to 80°C unless high temperature components are obtained from SiliCycle. Reacon temperatures must be

achieved using the apparatus described in this manual.

Pressure

SiliCycle MiniBlocks are not designed to withstand pressure build-up. Care should be taken to avoid pressure build-up when designing SiliCycle

MiniBlock synthesis procedures.

Components

Use only SiliCycle MiniBlock components purchased from, or approved by SiliCycle.

Document Convenons

The SiliCycle MiniBlock reactor is the central plaorm in SiliCycle’s advanced system for parallel

synthesis. SiliCycle MiniBlock reactors can be used to yield synthesis products for either high-throughput

or larger volume applicaons.

WARNING : is used to indicate the presence of a hazard which can cause personal

injury or death.

CAUTION : is used to indicate a potenal for damage to equipment

or synthesis results.

TECH TIP : is used to explain a product or operaonal nuance for a more eecve use of

the SiliCycle MiniBlock system.

2. General

The SiliCycle MiniBlock is designed to enable the chemist to achieve maximum product yield and purity,

while minimizing the potenal for cross-contaminaon.

The SiliCycle MiniBlock’s patented valve mechanism enables simultaneous boom drainage of all reacon vessels, aided by the use of vacuum

and pressure. Reacon products are then transferred into collecon vessels, or SPE tubes for puricaon.

Ancillary components are used to achieve reacon agitaon and temperature control for the SiliCycle MiniBlock system.

Height Width Depth Weight

5” (13 cm)7” (18 cm)5” (13 cm)6.4 lbs (2.9 kg)

Table 1: MinBlock Physical Descripon

Figure 1: SiliCycle MiniBlock

SiliCycle MiniBlock® User Guide

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2.1. The SiliCycle MiniBlock Reacon Tubes

SiliCycle MiniBlock Reacon Tubes are designed as simple yet robust vessels for chemical synthesis. They consist of glass or polypropylene reacon

tubes containing a 20 μm frit for solids ltraon.

Figure 2: Reacon

Tube Components

Figure 3: SiliCycle

MiniBlock Components

Polyethylene

Reacon Tube Cover Plate

Septum Layer

Upper Alignment Plate

Lower Alignment Plate

Blue Teon®

Heat Shrink Sleeve

Large Alignment Pin

Small Alignment Pin

Reacon Tube

20 µm Frit

Pinch Tube

Female Luer Fing

Male Luer Fing

Glass reacon tubes also have a Teon® heat shrink sleeve at the luer p to improve sealing. When using toluene, or other solvents to which

polypropylene is not fully resistant, glass reacon tubes should be used instead.

Figure 4: Glass Reacon Tube

With Teon® Heat Shrink Sleeve

0.5 0.50.5

Pinch-Tube Inserts are available in PFA Teon®. PFA Teon® inserts can be used at high temperatures, PFA ngs also provide good chemical

resistance, parcularly to toluene. (Figure 5).

The Reacon Tubes are sealed at the boom by compressing the Pinch-Tubes, which project through the SiliCycle MiniBlock (Figure 6). This closure

is achieved for all Reacon Tubes simultaneously with a single turn of the T-handle valve key (Figure 7).

Reacon Tube

PFA Teon ©

Grey Fings

Figure 6: Valve Mechanism

in Closed Posion

Figure 7: SiliCycle MiniBlock

with Valve Key

Figure 5: Types of Pinch-Tube Inserts

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2.2. SiliCycle MiniBlock Conguraons

The base SiliCycle MiniBlock comes as standard with 48 female luer ngs in the base. SiliCycle MiniBlock can be adapted

to any of four basic conguraons:

Reacon Tubes

per SiliCycle MiniBlock

Reacon Tube

Volume (mL)Reacon Tube Material Collecon Format

48 (Blue Block)4Polypropylene or Glass 48 or 96 posions

48 (Red Block)4Polypropylene or Glass 48 or 96 posions

24 (Green Block)10 Glass 24 posions

12 (Silver Block)20 Glass 12 posions

6 (Gold Block)40 Glass 6 posions

Table 2: SiliCycle MiniBlock Conguraons

SiliCycle MiniBlock conguraons, together with the reacon tubes and color-coding are depicted in Figure 8.

Glass reacon tubes are provided with a blue Teon® heat-shrink sleeve at the luer p. This is to improve sealing against the female luer ng:

(Figure 4). Insert glass reacon tubes into Pinch-Tube Inserts gently and carefully to avoid snagging or damaging the Teon® heat-shrink sleeve.

Figure 8: Reacon Tube Conguraons

Blue

Silver

4 mL 4 mL

10 mL

20 mL

40 mL

Red

Gold

Green

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