EP1339486A2 - Reseau d'autoclaves - Google Patents

Reseau d'autoclaves

Info

Publication number
EP1339486A2
EP1339486A2 EP01982380A EP01982380A EP1339486A2 EP 1339486 A2 EP1339486 A2 EP 1339486A2 EP 01982380 A EP01982380 A EP 01982380A EP 01982380 A EP01982380 A EP 01982380A EP 1339486 A2 EP1339486 A2 EP 1339486A2
Authority
EP
European Patent Office
Prior art keywords
autoclave
pressure
modules
reaction
control chamber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP01982380A
Other languages
German (de)
English (en)
Inventor
Boris E. Bosch
Thomas Riermeier
Uwe Dingerdissen
Gerhard Geiss
Norbert Stoll
Martin Krohn
Robert Lemke
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Evonik Operations GmbH
Original Assignee
Degussa GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Degussa GmbH filed Critical Degussa GmbH
Publication of EP1339486A2 publication Critical patent/EP1339486A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04—Pressure vessels, e.g. autoclaves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00162—Controlling or regulating processes controlling the pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00306—Reactor vessels in a multiple arrangement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00389—Feeding through valves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00477—Means for pressurising the reaction vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00479—Means for mixing reactants or products in the reaction vessels
    • B01J2219/00484—Means for mixing reactants or products in the reaction vessels by shaking, vibrating or oscillating of the reaction vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00495—Means for heating or cooling the reaction vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00585—Parallel processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00601—High-pressure processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/0068—Means for controlling the apparatus of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/0068—Means for controlling the apparatus of the process
    • B01J2219/00686—Automatic
    • B01J2219/00689—Automatic using computers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/0068—Means for controlling the apparatus of the process
    • B01J2219/00702—Processes involving means for analysing and characterising the products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00718—Type of compounds synthesised
    • B01J2219/00745—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B40/00—Libraries per se, e.g. arrays, mixtures
    • C40B40/18—Libraries containing only inorganic compounds or inorganic materials
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B60/00—Apparatus specially adapted for use in combinatorial chemistry or with libraries
    • C40B60/14—Apparatus specially adapted for use in combinatorial chemistry or with libraries for creating libraries

Definitions

  • the invention relates to a modular autoclave array and a method for determining suitable reaction conditions and mixtures for chemical syntheses on an industrial scale.
  • catalysts are predominantly used today. By reducing the activation energy required for the chemical process, these enable a substantial improvement in the material conversion. Due to the wide range of applications, there is a need to find and optimize new catalysts and catalytic reactions. The efficiency of the catalysts depends not only on their structure but also on process parameters such as pressure, temperature, the solvent and in particular also on Catalysts. As a result, the search and optimization of catalysts and catalytic processes result in a large number of test runs to be carried out under defined and reproducible reaction conditions.
  • the object of the present invention is therefore to provide a device for quickly determining suitable reaction conditions and suitable reaction batches for chemical syntheses with low consumption of substances to be used, and the associated method.
  • a scalable autoclave array which consists of autoclave modules, each consisting of a reactor jacket, which is sealingly attached over a reaction vessel, and which, via independently controllable autoclave valves, consists of a pressure control chamber containing a pressure sensor, which has at least one controllable valve with at least one Gas supply and at least one gas outlet is connected, can be filled with gas.
  • the autoclave modules of the device consist of a reactor jacket, which is connected to the associated autoclave valve, and the reaction vessel itself, which can be attached tightly to the jacket. The tight connection between the reactor jacket and the reaction vessel can be achieved via pressure, for example by means of a screw thread.
  • reaction vessel being able to be inserted into a holder which can be screwed to the reactor jacket.
  • reaction vessel used can be a simple, inexpensive, interchangeable container. It is irrelevant whether the container is used as a one-way or reusable reaction vessel B used as a reaction vessel with crimp or septa lid closable glasses, as they are often used for analytical purposes
  • sealing materials can be used as sealing materials.
  • Teflon or Viton have been used
  • the reactor jacket of the autoclave modules is connected to at least one controllable autoclave valve. Gas-tight valves with a small dead volume, such as binary switches, are preferred.
  • the reactor jacket can contain a closable channel for filling the autoclave module with the reaction batch or for removing the reaction products Such a channel is particularly advantageous if the process is to be carried out under inert gas conditions.
  • the reaction batch can also be introduced into the reaction vessel
  • the filling or the removal of substances for the direct analysis of the reaction products from the autoclave module can be automated, for example by a pipetting robot
  • the autoclave modules can be temperature-controlled.
  • conventional heating or cooling baths can be used
  • a modular autoclave array construction has proven to be advantageous, in which the temperature is controlled by means of a channel system embedded in the reactor jacket, through which a coolant or heating medium can be passed.
  • the channel system can be formed from holes in the reactor jacket. If the individual autoclave modules are tightly connected to one another, depending on the shape of the bore, cross-module channel systems can be easily created. It is preferred if the bore is as close as possible to the inside of the reactor jacket in order to ensure rapid temperature control of the reaction vessel.
  • scalable autoclave lines are assembled from the autoclave modules with a cross-module channel system for temperature control via plug connections.
  • Each autoclave line can thus be temperature-controlled independently of one another.
  • a great advantage of such a channel system is the rapid temperature control of the reaction vessels, both heating and cooling of the autoclave modules being possible.
  • the number of modules used remains freely selectable, the autoclave array device is thus easily scalable.
  • the individual autoclave modules are each connected to a pressure control chamber via an autoclave valve that can be controlled independently of one another.
  • the desired set pressure can be set in the pressure control chamber via the meterable gas supply.
  • the desired pressure can be generated in the autoclave modules independently of one another. It is advantageous if the reaction space consisting of the reaction vessel volume up to the autoclave valve is small compared to the volume of the pressure control chamber.
  • the pressure setting in the individual autoclave modules can be repeated cyclically. With the help of this time-multiplexed setting of the reaction pressure, a constant reaction pressure can be set by readjusting if necessary. Isobaric reaction control is possible without additional effort.
  • a reference volume chamber is present between the individual autoclave valves and the pressure control chamber, which is connected to the pressure control chamber via controllable valves.
  • the reference volume chamber has a precisely defined one Volume, the reference volume
  • the reference volume chamber and the autoclave modules can be filled with gas via the controllable open valves from the pressure control chamber up to a predefinable target pressure.
  • the pressure setting of the individual autoclave modules can be carried out independently of one another.
  • the reference volume chamber can the pressure control chamber a freely selectable reaction gas target pressure can be set.
  • an autoclave module valve can be opened w earth, the pressure difference in the reference volume chamber is determined by a pressure sensor that measures the actual pressure after opening the autoclave valve
  • the consumption of reaction gas for each autoclave module can be tracked independently of each other in a time-resolved manner.
  • a scalable autoclave array constructed in this way is particularly suitable for the parallel analysis of reactions with at least one gaseous starting material
  • FIG. 1 shows an embodiment of the autoclave array according to the invention with a reference volume chamber
  • the autoclave array used in this embodiment consists of an autoclave cell with 1 x 8 individual reactors, the autoclave modules (1) - (8).
  • the individual autoclave modules are connected to the via a line system (10) via an autoclave module valve (11) - (18)
  • Reference volume chamber (19) connected The actual pressure is measured via a pressure sensor (20) on the reference volume chamber (19).
  • the reference volume chamber (19) is connected to the pressure control chamber via a valve (9)
  • Pressure control chamber is determined by means of a pressure sensor (22).
  • the pressure control chamber (21) is also connected via a valve (24) with an inert gas reservoir (27), via a valve (25) with a reaction gas reservoir (28) and via a valve (23) with a Gas outlet ⁇ / akuumsystem (26) through the line system (10) connected
  • a continuous measurement of the pressure drop is possible with additional pressure sensors which are attached between the autoclave valve and the reactor jacket.
  • additional pressure sensors which are attached between the autoclave valve and the reactor jacket.
  • the introduction of a pressure sensor into the autoclave module itself is also conceivable, but technically more complex
  • the setpoint pressure is set via a gas supply that can be metered through a valve and via a gas outlet that can be metered, whereby a vacuum pump can also be connected.
  • a gas supply that can be metered through a valve and via a gas outlet that can be metered, whereby a vacuum pump can also be connected.
  • Several independently adjustable gas supplies and gas outlets can also be connected to the pressure control chamber
  • an independent inert gas supply is advantageous.
  • the device can be placed under inert gas
  • the individual autoclave modules can each be provided with a stirring device for mixing the reaction batches.
  • Electromagnetic stirring or stirring via a vibrating rod is preferred, which consists of a flexible tube closed on the lower side, which is tightly attached via an opening in the reactor jacket Through the opening, the vibrating rod can be set in motion with a slightly curved rotating rod reaching into the tube.
  • the results obtained are due to the autoclave array construction, the process management and the measurement methodology on technical processes transferable, whereby the often complex and expensive procedural scaling processes are shortened or completely avoided.Furthermore, the necessary material expenditure and the associated amount of waste products in the experimental evaluation of a chemical reaction are very low.
  • the autoclave module volume of less than 100 ml is unproblematic, and reactions in Modules with a volume of 1 ml can be reproducibly performed.
  • Another advantage of the device according to the invention is that the autoclave array can produce reproducible reaction conditions in a very wide temperature range and pressure range.
  • all autoclave modules can be operated via only one pressure control chamber or via a reference volume chamber can be filled with gases
  • the combination of pressure control chamber and reference volume chamber enables the pressure setting and the pressure difference measurement to be carried out very precisely and quickly lie, this is particularly advantageous for the investigation of small reaction batches
  • Another object of the invention is a method for the parallelized investigation of chemical reactions using the claimed autoclave array devices
  • reaction batches can be placed in the reaction vessel before being attached to the reactor jacket. If there is a closable channel in the reactor jacket, chemical substances can also be added before or during the reaction to be investigated, if necessary in countercurrent
  • the pressure setting in the individual autoclave modules, the valves of which are open, is carried out via the controlled opening of the gas supply and gas outlet until the desired setpoint pressure has been reached in the accessible space.
  • the real pressure is determined via a pressure sensor located in the pressure control chamber and with the specified setpoint pressure adjusted If the measured real pressure is equal to the set pressure, the autoclave valves are closed. The cycle is repeated in the other autoclave modules to set the pressure
  • time-multiplexed pressure regulation takes place in the individual autoclave modules.
  • the respective target pressure in the pressure control chamber is set according to a predefinable pressure program, after which the gas supply and the gas outlet are shut off
  • pressure compensation between the pressure control chamber and The autoclave module and the regulation of the autoclave module valve are then adjusted to the pressure in the module in accordance with the specified pressure program.
  • the sequence is repeated for the individual autoclave modules, then a new pressure regulation cycle can begin
  • the method according to the invention thus comprises the following process steps a) introduction of individual reaction batches into the autoclave modules, b) successive setting of the target pressures in the respective autoclave modules, c) time-multiplex regulation of the pressures in the autoclave modules, relaxation of the gas pressure in the device and removal of the reaction products for analysis
  • the actual pressure is additionally determined after regulating the pressure in the autoclave module, with the gas supply and gas outlet sealed off.
  • the gas volume that has flowed into the autoclave module is then determined at the given temperature from the difference between the measured actual pressure and the setpoint pressure chemical conversion is advantageous, in which at least one gaseous starting material enters.
  • the reaction gas is fed into the autoclave via the pressure control chamber
  • the gas consumption measurement is carried out via a reference volume chamber connected between the pressure control chamber and the autoclave modules.
  • the setpoint pressure is set via the pressure control chamber when the autoclave module valves are closed the actual pressure after pressure equalization between the reference volume chamber and the autoclave module takes place via a pressure sensor built into the reference volume chamber
  • the pressure control chamber represents a defined gas volume in which the setpoint reaction pressures for the 8 autoclaves to be set in the reference volume chamber and in the pressure control chamber are iteratively adjusted while the compensation process between the autoclave and reference volume is still running.Afterwards, the valve between the reference volume chamber and the pressure control chamber transfers the pressure to the former and the The process is repeated cyclically
  • the gas consumption measurement is determined as the integral of the pressure differences describing the gas consumption over the reaction time for each individual reactor
  • the device is evacuated via a vacuum pump connected to the pressure control chamber and then charged with inert gas via a gas supply. The process can be repeated several times. If the autoclave module valves are open, then Inert gas countercurrent is filled via a closable channel embedded in the reactor jacket, the channel is then closed and the autoclave module valve is sealed off. The reaction batch is now under inert gas in the autoclave module. The device can then, if desired, continue with inert gas for pressure regulation or with a separately supplied reaction gas After completion of the reaction, the device can be placed under inert gas again.
  • a sampling of the reaction products can in turn be opened via the reactor jacket channel at etem autoclave module valve in the inert gas counterflow It is also possible to take samples from the individual autoclave modules during the reaction. To do this, however, the gas pressure in the respective autoclave must be released via the gas outlet, then a sample can be taken via the channel in the reactor jacket, if necessary in counter gas flow.
  • the examples of examined reactions presented below were carried out with an autoclave array according to FIG. 1.
  • the stainless steel autoclave modules used had a reaction volume of 3 ml.
  • Jars with crimp closures are used as reaction vessels.
  • the individual autoclave modules were tightly assembled into a 1x8 autoclave line.
  • the temperature is controlled via a channel system embedded in the reactor jacket with a medium that can be heated by a thermostat.
  • the safe, intensive and modulable mixing of the reactants is achieved by indirect magnetic stirring by means of rotary field transmission through the non-magnetic autoclave bottom.
  • the autoclaves Easy access to the samples after the reaction with contamination to be avoided and a coupling to analytical processes is ensured by designing the autoclaves as rotationally symmetrical one-way reaction vessels (100) in a sleeve (101) screwed into the reactor jacket (FIG. 2). Securability in the form of an evacuation of the system and the possibility of flooding with an inert gas is ensured by a short-circuit function of the pressure control system or the reference volume.
  • the reaction pressure setting with the reactant gas is ensured with the help of the pressure sensors in the pressure control system and the reference volume via a combination of pressure control chamber - reference volume chamber - autoclave module valve.
  • a gas-tight binary switch with a small dead volume and small opening and closing tents is used as the autoclave module valve
  • Reproducible conditions can be achieved with such an autoclave array in a temperature range from -50 to 200 ° C and a pressure range from 0 to 200 bar
  • the individual reaction batches are examined in the autoclave array according to the following process program: a) temperature control of the autoclave modules b) repeated flooding and securing of the entire gas supply system with inert gas (Ar), c) flooding of the autoclave modules with inert gas (Ar) in countercurrent d) opening the screwable reactor jacket duct .
  • reaction batch consisting of 15 ml of AAZSE (0.5 M in MeOH) and 1.5 ml of a catalyst solution of Rh (COD) 20Tf / R, R-EtDuPHOS ( 1 1, 1 in MeOH) and 21, 0 ml MeOH combined under inert gas and reacted in a 50 ml autoclave at a pressure of 5 bar and a temperature of 25 ° C.
  • the reaction time was 2 hours conversion 100%, reactant content enantiomer 1 96, 2845 area%, enantiomer 2 1, 8142 area%, ee 96.3%
  • the results of the investigated reaction in the autoclave array device according to the invention can accordingly be transferred to larger reaction vessels

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un réseau d'autoclaves modulable pour l'analyse de réactions chimiques. Le réseau d'autoclaves selon l'invention est constitué de modules autoclaves qui sont chacun constitués d'une enveloppe de réacteur fixée étanche sur un récipient de réaction et qui peuvent être remplis de gaz indépendamment les uns des autres par l'intermédiaire de soupapes d'autoclave réglables à partir d'une chambre de régulation de pression qui contient un capteur de pression et qui est reliée par l'intermédiaire d'au moins une soupape réglable à au moins une arrivée de gaz et à au moins une sortie de gaz.
EP01982380A 2000-10-02 2001-09-28 Reseau d'autoclaves Withdrawn EP1339486A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10049078A DE10049078A1 (de) 2000-10-02 2000-10-02 Autoklaven-Array
DE10049078 2000-10-02
PCT/EP2001/011249 WO2002030557A2 (fr) 2000-10-02 2001-09-28 Reseau d'autoclaves

Publications (1)

Publication Number Publication Date
EP1339486A2 true EP1339486A2 (fr) 2003-09-03

Family

ID=7658614

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01982380A Withdrawn EP1339486A2 (fr) 2000-10-02 2001-09-28 Reseau d'autoclaves

Country Status (6)

Country Link
US (1) US20040013565A1 (fr)
EP (1) EP1339486A2 (fr)
JP (1) JP2004510575A (fr)
AU (1) AU2002213979A1 (fr)
DE (1) DE10049078A1 (fr)
WO (1) WO2002030557A2 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004039210C5 (de) * 2004-08-12 2012-11-15 Rudolf Wild Gmbh & Co. Kg Verfahren zur Bewertung der Produkthaltbarkeit in einem Packmittel
US7807109B2 (en) * 2007-05-14 2010-10-05 Freeslate, Inc. Parallel batch reactor with pressure monitoring
US20080286170A1 (en) * 2007-05-14 2008-11-20 Symyx Technologies, Inc. Parallel batch reactor
EP2160237A2 (fr) * 2007-05-14 2010-03-10 Symyx Solutions Inc. Réacteur à fonctionnement discontinu en parallèle
US7655191B2 (en) * 2007-05-14 2010-02-02 Symyx Solutions, Inc. Methods for chemical reactions in a parallel batch reactor

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1164381B (de) * 1961-03-18 1964-03-05 Bayer Ag Reaktorsystem
CH644828A5 (en) * 1979-11-10 1984-08-31 Deppen Jean Claude Process for the manufacture of permeable prefabricated components and device for making use of this process
US4670404A (en) * 1985-04-22 1987-06-02 Fike Corporation Micro-scale chemical process simulation methods and apparatus useful for design of full scale processes, emergency relief systems and associated equipment
US4990076A (en) * 1989-05-31 1991-02-05 Halliburton Company Pressure control apparatus and method
NO304355B1 (no) * 1997-02-20 1998-12-07 Sinvent As Multi-autoklav for metodisk, automatisert syntese av zeolitter og andre forbindelser
DE19835914A1 (de) * 1998-08-07 2000-02-17 Basf Ag Verfahren zum Dosieren eines flüssigen, gasförmigen oder in überkritischem Zustand vorliegenden Mediums in einen Druckreaktor
US6306658B1 (en) * 1998-08-13 2001-10-23 Symyx Technologies Parallel reactor with internal sensing
AU2177700A (en) * 1998-12-15 2000-07-03 Union Carbide Chemicals & Plastics Technology Corporation Apparatus and methods for combinatorial chemical analysis

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0230557A3 *

Also Published As

Publication number Publication date
JP2004510575A (ja) 2004-04-08
WO2002030557A3 (fr) 2002-08-08
US20040013565A1 (en) 2004-01-22
AU2002213979A1 (en) 2002-04-22
DE10049078A1 (de) 2002-04-18
WO2002030557A2 (fr) 2002-04-18

Similar Documents

Publication Publication Date Title
DE69527613T2 (de) Mikroreaktor für ein modulares System
DE19830607C2 (de) Verfahren zum Nachweis eines Produktes im Abstrom eines katalytischen Materials einer Vielzahl von katalytischen Materialien
DE69428048T2 (de) Batch-betriebener mikrowellenreaktor
DE19529099C2 (de) Vorrichtung zur Serien-Kultivierung von Mikroorganismen bzw. Zellen in begasten Flüssigkeitssäulen
DE69908336T2 (de) Parallel-reaktor mit interner fühlung und verfahren zu dessen verwendung
EP1256378A2 (fr) Dispositif et procédé pour la mise en oeuvre d'expériments en parallèle
DE69833620T2 (de) Vorrichtung für die Anwendung in der Mehrfachsimultansynthese von allgemeinen Verbindungen
EP4028156B1 (fr) Dispositif et procédé pour étudier des processus chimiques
DE2904644B2 (de) Vorrichtung zum Präparieren, insbesondere Markieren, von biologischen Proben
EP2046493B1 (fr) Dispositif et procédé de manipulation de mélanges à composants multiples
EP0010571A1 (fr) Procédé et dispositif pour réaliser des réactions (bio)chimiques et des opérations d'unité en systèmes fluide/fluide
DE102004003925A1 (de) Universeller kontinuierlich betriebener Säulenreaktor für chemische Synthesen vom Labor- bis in den Pilotmaßstab
EP3930887A1 (fr) Automatisation de processus de laboratoire par un dispositif d'assistance à des processus de laboratoire
EP1339486A2 (fr) Reseau d'autoclaves
EP1379622B1 (fr) Procede et dispositif de culture et/ou de repartition de particules
EP3866963A1 (fr) Dispositif et procédé d'examen de réactions
DE60126023T2 (de) Sequentielles Reaktionsystem
DE69605554T2 (de) Gefäss für chemische synthesen und dieses verwendende system
DE102005049152A1 (de) Verfahren und Vorrichtung zur Bereitstellung einer Substanz für die Analyse von Isotopenverhältnissen
DE102007063440A1 (de) Screeningsystem zur Durchführung und direkten Analyse von biologischen, biochemischen und chemischen Synthese- und Umsetzungsreaktionen
EP1287328A1 (fr) Dispositif et procede de traitement de prelevements lies a un substrat
DE19861316B4 (de) Anordnung zum Testen der katalytischen Aktivität von einem Reaktionsgas ausgesetzten Feststoffen
DE10260690B4 (de) Abdeckung für eine Vorrichtung, damit abgedeckte Vorrichtung und Verfahren zur parallelen, automatisierten Kultivierung von Zellen unter technischen Bedingungen
EP1392813B1 (fr) Bioreacteur comportant au moins deux chambres de reaction
DE2655265C3 (de) Verfahren zur automatischen Vorbereitung von aus Zellsuspensionen bestehenden Proben zum Zwecke der nachfolgenden Bestimmung intra- und/oder extrazellulärer Stoffe durch eine kontinuierlich aufeinanderfolgende Behandlung einer Mehrzahl von Proben

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20030502

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR

AX Request for extension of the european patent

Extension state: AL LT LV MK RO SI

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20050203