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Содержание QUEST 205

Страница 1: ...service in house repair center WE BUY USED EQUIPMENT Sell your excess underutilized and idle used equipment We also offer credit for buy backs and trade ins www artisantg com WeBuyEquipment REMOTE IN...

Страница 2: ...ARGONAUT TECHNOLOGIES Part Number 102965 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 3: ...Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 4: ...s 2 1 User Supplied Items 2 1 InstallationGlossary 2 2 Settingup the Quest 205 Synthesizer 2 2 Connecting the Interface Harness to the Controller Unit 2 3 Connecting the Bottle Cap Assembly 2 3 Connec...

Страница 5: ...10 Parameter Setting Buttons 3 10 START STOPButton 3 10 Agitator Control Buttons 3 11 Agitation Needle Valve 3 11 Controller Unit Gas and Power Connections 3 12 SystemGas 3 12 Electrical Outlet 3 12 P...

Страница 6: ...22 DrainingSynthesisProducts to CollectionFlasks 4 22 5 Maintenance 5 1 Post SynthesisCleaning 5 1 Manifold Maintenance 5 3 6 Glossary 6 1 7 Controller Unit Display Screens 7 1 Sign OnScreen 7 1 Firmw...

Страница 7: ...nt and Solution Preparation 10 2 RV Removal Instrument Cleaning and RV Installation 10 5 Reductive Amination 10 6 Filling the Dead Volume Between the RV frit and the Lower Manifold Drain Valve 10 6 Ad...

Страница 8: ...cts herein to improve reliability fimction or design Argonaut Technologiesdoes not assume any liability arising out of the application or use of any product or circuit described herein neither does it...

Страница 9: ...performing solid phase or solution phase reactions Section 5 Maintenance Provides step by step instructions on maintenance procedures for optimum instrument performance Section 6 Glossary Defines term...

Страница 10: ...llel using the manual rotary valves Reagents are added via luer ports located at the top of each Reaction Vessel The Controller Unit contains the controls to set the reaction temperature heating durat...

Страница 11: ...Teflon Proprietary vertical oscillation mechanism 40 C to 130 C 5 requires recirculating chiller for temperature control below ambient Accommodates 14 20 19122 24140 29126 and 29142 pear shaped or rou...

Страница 12: ...warranty period Additional expenses covered by the Warranty are 1 Labor and materials for covered items 2 Shipping of repaired systems and accessories back to the Customer after service 3 Shipment cos...

Страница 13: ...preventative maintenance as specified in the Quest 205 User Manual 4 Damage caused by non conformance to recommended instrument operation procedures 5 Any product on which the serial number has been...

Страница 14: ...must be filled out and mailed after installation is complete To qualify for warranty repair first contact the appropriate repair center detailed in this chapter Contact Information Interference Infor...

Страница 15: ...by the manufacturer the protection provided by the equipment may be impaired Safety This equipment has been tested and found to comply with the requirements as set forth in the European Immunity Stan...

Страница 16: ...ssful installation and safe use of the Quest 205 WARNING If the equipment is used in a manner not specified by the manufacturer the protection provided by the equipment may be impaired This equipment...

Страница 17: ...tenz 2 Switzerland Phone 41 61 465 9898 Fax 41 61 465 9899 Japan Argonaut TechnologiesK K MK Komachi Bldg 4 2 1 Kojimachi Chiyoda Ku Tokyo 102 Japan Phone 81 3 3234 4321 Fax 81 3 3234 4321 E Mail stan...

Страница 18: ...Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 19: ...Domestic Instruments or 2 5L capacity for International Instruments User Supplied Items If using a single gas source 55 60 psi house nitrogen supply or other high purity 99 98 inert gas If using dual...

Страница 20: ...as connections within the Quest 205 Controller Unit Setting up the Quest 205 Synthesizer 1 Clear a space about 2 114 feet 70 cm wide by 2 feet 60 cm deep in a fume hood for the Quest 205 Reactor Unit...

Страница 21: ...bushing should not be bound to the yellow ferrule as this can cause twisting of the Teflon tube during installation To release a bound bushing from a ferrule grasp the ferrule between the thumb and in...

Страница 22: ...towards the rear of the fume hood or taue it down to a convenient suot in the fume hood Connecting the Reactor Unit Manifold Tubes Six tubes three on each side of the Quest 205 must be connected to bu...

Страница 23: ...of the tube labeled MAN VENT into the red bulkhead fitting on the upper Reactor Unit labeled VENT Screw the other end of the MAN VENT tube into the female threaded port on the Upper Manifold in the m...

Страница 24: ...the buttons and raise the tray and tank 6 Attach the supplied Teflon tubing to the drain valve located on the waste tank Place the other end of the tubing into an appropriate waste container Setting...

Страница 25: ...e other quick disconnect fitting to the compressed air inlet on the rear panel of the Controller Unit c Push the fittings over the inlet ports until an audible click is heard from each fitting Connect...

Страница 26: ...k connect fitting onto the compressed air inlet on the rear panel of the Controller Unit until an audible click is heard Connecting Power to the Quest 205 1 Plug the power cord into the female recepta...

Страница 27: ...arked Pressure Wait about a minute for the bottle to pressurize In the Pressure position 9 psi gas flows from the Controller Unit into the solvent bottle via the pressure line WARNING Always vent the...

Страница 28: ...Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 29: ...nit has ports to connect lines from the Reactor Unit These lines from the Reactor Unit make up the Interface Harness and include the electrical metered gas 9 psi drain gas 30 psi solvent and two agita...

Страница 30: ...f RVs the ends of the Reaction Vessels press over the male fittings of both Upper and Lower Manifolds This along with the upper and lower RV clamp creates a leak tight seal for the Reaction Vessels He...

Страница 31: ...y a pneumatic cylinder The rod oscillates vertically when gas is supplied to either end of the pneumatic cylinder Valves in the Controller Unit alternately supply 30 psi gas to the bottom and top of t...

Страница 32: ...flon tubing which vents into the waste tank Set to Metered Gas allows 9 psi gas into the corresponding Upper Manifold common pathway Setting Control Valve 2 to UTILITY 2 attachesthe correspondingUpper...

Страница 33: ...waste Drain valves can be opened individually or in groups Waste Tank The Quest 205 is equipped with a rectangular plastic tank for waste collection The Waste Tank is equipped with a plug valve to whi...

Страница 34: ...op of the Reactor Unit controls gas flow to the membrane switchingthe membrane from open to closed In Addition the Upper Manifold contains individual mechanically actuated plungers above each Reaction...

Страница 35: ...or both Reactor Unit Sides A and B The Metered Gas Needle Valve is used to increase or decrease the gas flow rate once the Manifold Control Valves are set to deliver 9 psi gas to the Reaction Vessels...

Страница 36: ...and electronics boards LCD Screen and Keypad The Controller Unit LCD screen and keypad are used to set the reaction temperature temperature duration and agitationparameters LCD Screen The LCD screen...

Страница 37: ...t this temperature and indicate the volume in the 100mL Reaction Vessels Monitor Temperature Screen Displays the set point temperature of the Reaction Vessel banks the actual temperature remaining hea...

Страница 38: ...alue of the selected parameter Press the Down Parameter button down arrow to decrease the value of the selected parameter For information on the function of the Parameter Setting buttons in a particul...

Страница 39: ...to start mixing the reaction solution once the agitation parameters have been set on the Agitation Control screen For detailed informationon setting the agitation see Operating the Quest 205 Setting o...

Страница 40: ...ulated 55 60 psi source of clean dry compressed air The gas ports are located on the rear of the Controller Unit adjacent to the power switch and the electrical socket Quick connect fittings are used...

Страница 41: ...he fume hood and pointed away from the user A long Teflon line runs from the bottom of the Teflon cap This line is the pickup tube for the solvent in the bottle and should reach the bottom of the bott...

Страница 42: ...Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 43: ...n Verify that there is sufficient system gas at the supply Install a solvent bottle if necessary and a filter see Installing the Solvent Bottle in Section 2 Install the rectangular waste tank undernea...

Страница 44: ...3 Using the 7 64 hex driver loosenthe upper Reaction Vessel clamps The clamps are located at thejunction of the Reaction Vessels and the Upper Manifold 4 Raise the Upper Manifold WARNING Always vent...

Страница 45: ...ilt the Upper Manifold to keep it open This prevents the manifold from swinging back into the Reaction Vessels a Side A Tilt the Upper Manifold to the left b Side B Tilt the Upper Manifold to the righ...

Страница 46: ...l the luer port adapter insert it into the Upper Manifold Rotate the adapter in a clockwise direction until a slight resistance is felt and continue for an additional 4turn NOTE Over tightening of the...

Страница 47: ...and swing it into the closed position a Side A Tilt the Upper Manifold to the right b Side B Tilt the Upper Manifold to the left 10 Push the hinge pin attached by a cord to the Reactor Unit through t...

Страница 48: ...bank holds five Reaction Vessels All five Reaction Vessels do not need to be used in each synthesis If less than five Reaction Vessels are needed the unused Reaction Vessels can be shut off 1 If the...

Страница 49: ...low rate to each vessel is within lo If the previously closed position has low flow the dummy RV screw may not have been loosened enough Waste Tank 1 Ensure the waste tank is properly positioned under...

Страница 50: ...meters to minimize splashing of solution on the Upper Manifold male fittings This prevents the build up of resin andlor particulates in the her ports Three parameters are shown on the Agitation displa...

Страница 51: ...uid extraction is being done increase the stroke frequency and stroke velocity to increasethe mixing efficiency MixEvery parameter agitation needle valve NOTE It is advisable to keep the magnets in th...

Страница 52: ...r decrease the Upward parameter The Upstroke parameter automaticallychanges to reflect the new value set for Upward 5 Press the Agitator ONIOFF button located on the Controller Unit to start the mixin...

Страница 53: ...hen working near or on the Reactor Unit When heating the Reactor Unit becomes hot Allow the Reactor Unit to cool before attempting to access the Reaction Vessels Prior to starting a heating step set b...

Страница 54: ...This prevents against over pressurization of the system 4 Use the Forward and Back buttons to place the cursor over one of the digits of the setting in the RV Volume field NOTE There is a separate vo...

Страница 55: ...rom an existing set point by accessing the Set Temperature screen 11 The heaters turn off when the time has elapsed or they can be manually stopped To stop the heaters a Locate the cursor on the scree...

Страница 56: ...Vessels on a bank and prevents any crossover of Reaction Vessel contents from vessel to vessel NOTE The functions of the Manifold Control Valves are disabled when the Membrane Pressure switch is in t...

Страница 57: ...L PRESS e Wait about 1 minute for the bottle to pressurize WARNING Always place the solvent bottle in the vlastic safetv carrier 2 Toggle the Upper Manifold Membrane Switch to OPEN 3 Initialize the so...

Страница 58: ...erify that the waste tank is installed below the Reactor Unit 2 Toggle the Upper Manifold Membrane Switch to OPEN 3 Open the drain valves on the Lower Manifold by pushing down on the Drain Valve Lever...

Страница 59: ...LVENT CLOSED VENT 0CLOSED UTILITY 1 CONTROL VALVE 1 UTILITY 2 CONTROL VALVE 2 Figure4 8 Control Valves set to CLOSED and VENT NOTE Ensure the RVs and manifolds are clean before performing the followin...

Страница 60: ...trol Valve 2 will gently equalize the pressure and avoid bumping the solution see figure 4 8 2 Slowly remove the luer plug by rotating the plug while pulling it out WARNING Always wear safety glasses...

Страница 61: ...ves to CLOSED Adding Liquid Solvent or Reagents to an Air Sensitive Chemistry NOTE To monitor inert gas flow while adding liquid chemicals to an air sensitive reaction a bubbler can be attached to the...

Страница 62: ...ERED GAS on the side with the target Reaction Vessel 5 Insert the pierced septa luer plug into the luer port adapter of the target Reaction Vessel WARNING Ensure the tubing does not go below any liqui...

Страница 63: ...per Manifold Membrane Switch to the CLOSED position 18 Rotate the Quest 205 so that the target Reaction Vessel is easily accessible 19 Remove the transfer cannula from the target Reaction Vessels luer...

Страница 64: ...r in up position to will prevent agitation magnets from getting stuck in resin 1 Toggle the Upper Manifold Membrane Switchto OPEN 2 Vent the system to relieve any residual pressure that can cause spla...

Страница 65: ...ask 7 Set Control Valve lto CLOSED and Control Valve 2 to METERED GAS to pressurize the head space over the Reaction Vessels NOTE When collecting product use the 10 psi metered gas to provide the head...

Страница 66: ...Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 67: ...prior to draining the solvent 2 After the last solvent wash let the system drain for a couple of minutes to flush residual solvent out of the Reactor Unit A volatile solvent such as acetone may be des...

Страница 68: ...Upper Manifold and the Lower Drain Manifold Use a soft cloth and an appropriate solvent to wipe the fittings clean of any residue or particulates NOTE Do not allow any particulates to enter the throug...

Страница 69: ...the Manifolds to loosen Heating and cooling of the system accelerates this phenomenon Check and tighten the Upper Manifold bolts using the 7 64 hex wrench Check and tighten the Lower Manifold bolts u...

Страница 70: ...Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 71: ...ontroller Unit to the Reactor Unit Ferrule Yellow conical shaped piece which mates to the PPS fittingd Used for Teflon tube connections Flask Rack Holds up to five pear shaped or round flasks to colle...

Страница 72: ...sin and reagents are added for synthesis Reactor Unit Unit containing Teflon Reaction Vessels manual solvent and gas control valves and heating cooling and agitation components Teflon tubing Semi tran...

Страница 73: ...d explains how to use the Controller Unit buttons to select a screen and change the parameters Sign On Screen Quest 205 Argonaut Technologies Figure 7 1 Sign On Screen The Sign On screen identifiesthi...

Страница 74: ...re Version screen must be accessed through the Other Functions screen described later in this section Table 7 2 outlines the function of the Controller keypad buttons while at this screen Pressingthis...

Страница 75: ...s number is necessarily less than the agitation frequency value The Upward parameter controls the upstroke in the same manner as the Upstroke parameter but is expressed in terms of a percentage of the...

Страница 76: ...utton Results in MODE Set Temperature screen appearing FORWARD ACK Selectinga parameter on the screen PARAMETER Increasing or decreasingthe value of the chosen parameter STARTISTOP StartIStop Heaters...

Страница 77: ...le 7 4 outlines the function of the Controller keypad buttons while at this screen Pressing this button Results in MODE Monitor Temperature screen FORWARDIBACK Selecting a parameter on the screen Incr...

Страница 78: ...temperature of the reaction and whether the heaters are on or off Table 7 5 outlinesthe function of the Controller keypad buttons while at this screen Pressingthis button Results in MODE Other Functi...

Страница 79: ...available on the main screens Five other functions are available and are described below Only three of the five functions can be seen on the screen at one time The screen scrolls by pressing the Forw...

Страница 80: ...tton Results in MODE The screen choice 1 5 indicated by the cursor will be engaged Moving the cursor up or down to select one of the five screen options PARAMETER Moving the cursor up or down to selec...

Страница 81: ...hile at this screen Pressingthis button Results in MODE Returning to the Other Functions Screen FORWARD BACK Increasing or decreasing the display screen contrast PARAMETER Increasing or decreasing the...

Страница 82: ...s A and B 3 Success or failure of the transformer sensor 4 Success or failure of the two heaters A and B and 5 Status of the 16 valves While the self test is in progress a indicator at the top of the...

Страница 83: ...e Other Functions Screen STARTISTOP StartfStopHeaters screen appears Restore Defaults Screen AGITATOR ON This screen appears momentarily after the MODE button is pressed when option 5 Restore Defaults...

Страница 84: ...on press the Mode button to activate the option Table 7 9 outlines the function of the Controller keypad buttons while at this screen Pressingthis button Results in MODE Returning to previous screen S...

Страница 85: ...Quest 205 User Manual Revision B 72 03 98 8 Reactor Unit Plumbing Schematic Argonaut Technologies Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 86: ...Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com...

Страница 87: ...action bar next to the Reaction Vessels and slowly pull the magnet to the top of the RV Quest 205 Flask Rack P N 900199 Description The Quest 205 Flask Rack is used to support up to five 200 300 round...

Страница 88: ...reagents to the Weighing Funnel Transfer the Weighing Funnel from the balance to the Quest 205 Reactor Unit Unscrew the luer plug adapter and place the stout end of the weighing funnel into the her p...

Страница 89: ...ent flow to a Reaction Vessel remove the cabled hinged pin from the side of the upper manifold without the supply tubing and rotate out the upper manifold Lock the upper manifold by fully extending th...

Страница 90: ...t on the top of the Quest 205 Reactor Unit To monitor the inert gas delivery turn the Quest Control Valves to UTILITY 1 an METERED GAS The inert gas flow rate can be adjusted by turning the Metered Ga...

Страница 91: ...ulti flask adapter Securely fit the 1 blunt tip needle through the top of each multi flask adapter Then securely place the polypropylene valve onto the female luer fitting of the needle Rotate the pol...

Страница 92: ...the upper manifold her ports To deliver reagents under inert conditions turn the Quest Control Valves to UTILITY 1 and METERED GAS Adjust the inert gas flow by adjusting the Metered Gas Needle Valve c...

Страница 93: ...mL Reaction Vessels RVs on the Quest 205 Organic Synthesizer The RVs should be installed after the instrument is thoroughly cleaned see section A After the RVs are rinsed with MeOH add the R1 aniline...

Страница 94: ...The results reported in Table 3 Page 10 are representative and may vary based on the purity of the actual reagents used for this synthesis Instrument and Solution Preparation i R1 substitutedaniline...

Страница 95: ...n62 mL MeOH 660 7pL in13mL MeOH 790 9 pL in 13mL MeOH 766 4pL in13mL MeOH 692 7 pL in13mL MeOH 766 4 pL in13mL MeOH 586 4 mg 2x 31 mL EtOH 130mL 65 mL 90 mL 360 mL 12g cartridge Round Bottom Flask 250...

Страница 96: ...g with the Quest 205 Prior to Starting the Synthesis Read the Quest 205 User Manual Verify that the Quest was installed according to the Quest Installation Procedure in the Quest 205 User Manual For s...

Страница 97: ...en the RVs from the lower clamp by twisting the RVs upwards Once the RVs are free from the lower clamp remove the RVs from the Quest Remove the magnets by either turning the RVs upside down or by usin...

Страница 98: ...wer Manifold Drain Valve This procedure provides instructions on filling the dead volume between the bottom of the Reaction Vessel frit and the lower manifold drain valve with solvent This ensures tha...

Страница 99: ...ubstituted benzaldehydesMeOH to the RVs in the same manner Table 2 illustrates the RV reagent scheme After reagent addition snugly screw in the luer plugs for each RV to ensure a tight seal 1 4 I Anil...

Страница 100: ...the LCD displays the SET TEMPERATUREmenu Enter the following parameters for Bank A A 64C 3 00 OFF B 100C 0 00 OFF RVs A 20mL B 20mL 7 The heating duration and temperature can be adjusted by moving th...

Страница 101: ...e temperature and time parameters 11 Reflux the reaction for three hours at 64 C The heater will turn off after the when the heater program is complete Allow the reaction bank to cool to room temperat...

Страница 102: ...occur 5 Adjust the agitation stops so that the magnets in the RVs are approximately 1 cm below the solvent level in the RVs and turn the agitation on 6 Program the heater parameters by pressing the Co...

Страница 103: ...the lower luer male fitting on Bank B Place five tared 250 mL round bottom flasks into the flask rack and secure it into place Remove the waste tank and lower the waste tray to the lowest setting On...

Страница 104: ...tion 60 mL or 75 mL SPE cartridge optional 1 Prepare five 60 mL or 75 ml SPE cartridges with fiits with 12 g of neutral aluminum oxide bottom layer and 7 g of MgS04 top layer Place a small amount of g...

Страница 105: ...s maximum let the organic layer sit for ten minutes and open up the polypropylene valves to gravity drain the product 6 Let the organic layer sit for ten minutes and drain it directly into the 250 mL...

Страница 106: ...and luer plug adapters Dry the RVs by rotating the Quest Control Valves to DRAIN GAS and CLOSED with the lower manifold drain levers opened This allows the RVs to dry thoroughly to remove any residual...

Страница 107: ...e to remove residue fiom the reaction 5 Replace the luer plugs and luer plug adapters Dry the RVs by rotating the Quest Control Valves to DRAIN GAS and CLOSED with the lower manifold drain levers open...

Страница 108: ...e ReductiveAmination C Hl5NO C 4H15N C H13N0 Exacfd 83 Exact iiass 213 12 Exact lg712 Exact a s s 199 10 Mol Wt 183 25 Mol Wt 213 28 Mol Wt 197 28 Mol Wt 199 25 Figure 3 Structures of amine products A...

Страница 109: ...m 10H Ar H 4 34 s 2 H CH2 4 03 br s 1H NH PPm Compound 12 HPLC retention time 4 47 min H NMR CDC13 300 MHz 6 7 38 7 14 6 88 6 86 6 74 6 63 m 9 H Ar H 4 25 s 2 H CH2 3 79 s 3 H CH3 3 32 s 1H NH ppm Co...

Страница 110: ...service in house repair center WE BUY USED EQUIPMENT Sell your excess underutilized and idle used equipment We also offer credit for buy backs and trade ins www artisantg com WeBuyEquipment REMOTE IN...

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