JP3066862B2 - Automatic synthesizer - Google Patents

Automatic synthesizer

Info

Publication number
JP3066862B2
JP3066862B2 JP10269181A JP26918198A JP3066862B2 JP 3066862 B2 JP3066862 B2 JP 3066862B2 JP 10269181 A JP10269181 A JP 10269181A JP 26918198 A JP26918198 A JP 26918198A JP 3066862 B2 JP3066862 B2 JP 3066862B2
Authority
JP
Japan
Prior art keywords
reaction
block
reflux
reaction vessel
automatic synthesizer
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.)
Expired - Fee Related
Application number
JP10269181A
Other languages
Japanese (ja)
Other versions
JPH11165063A (en
Inventor
隆英 平野
隆明 井上
豊 蔵谷
顕一 北村
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.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
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 Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP10269181A priority Critical patent/JP3066862B2/en
Publication of JPH11165063A publication Critical patent/JPH11165063A/en
Application granted granted Critical
Publication of JP3066862B2 publication Critical patent/JP3066862B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F1/00Tubular elements; Assemblies of tubular elements
    • F28F1/02Tubular elements of cross-section which is non-circular
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/08Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being otherwise bent, e.g. in a serpentine or zig-zag
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/08Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being otherwise bent, e.g. in a serpentine or zig-zag
    • F28D7/082Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being otherwise bent, e.g. in a serpentine or zig-zag with serpentine or zig-zag configuration
    • F28D7/085Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being otherwise bent, e.g. in a serpentine or zig-zag with serpentine or zig-zag configuration in the form of parallel conduits coupled by bent portions
    • F28D7/087Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being otherwise bent, e.g. in a serpentine or zig-zag with serpentine or zig-zag configuration in the form of parallel conduits coupled by bent portions assembled in arrays, each array being arranged in the same plane
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277Apparatus
    • B01J2219/00279Features relating to reactor vessels
    • B01J2219/00281Individual reactor vessels
    • B01J2219/00283Reactor vessels with top opening
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277Apparatus
    • B01J2219/00279Features relating to reactor vessels
    • B01J2219/00281Individual reactor vessels
    • B01J2219/00286Reactor vessels with top and bottom openings
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277Apparatus
    • B01J2219/00279Features relating to reactor vessels
    • B01J2219/00306Reactor vessels in a multiple arrangement
    • B01J2219/00308Reactor vessels in a multiple arrangement interchangeably mounted in racks or blocks
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277Apparatus
    • B01J2219/00279Features relating to reactor vessels
    • B01J2219/00306Reactor vessels in a multiple arrangement
    • B01J2219/00308Reactor vessels in a multiple arrangement interchangeably mounted in racks or blocks
    • B01J2219/0031Reactor vessels in a multiple arrangement interchangeably mounted in racks or blocks the racks or blocks being mounted in stacked arrangements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583Features relative to the processes being carried out
    • B01J2219/00585Parallel processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583Features relative to the processes being carried out
    • B01J2219/0059Sequential processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583Features relative to the processes being carried out
    • B01J2219/00596Solid-phase processes
    • CCHEMISTRY; METALLURGY
    • C40COMBINATORIAL TECHNOLOGY
    • C40BCOMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B60/00Apparatus specially adapted for use in combinatorial chemistry or with libraries
    • C40B60/14Apparatus specially adapted for use in combinatorial chemistry or with libraries for creating libraries

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Geometry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Heat-Exchange Devices With Radiators And Conduit Assemblies (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Control Of Temperature (AREA)

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、化合物の合成を行
う装置に関し、特に複数の化合物を同時合成する自動合
成機に関する。
The present invention relates to an apparatus for synthesizing a compound, and more particularly, to an automatic synthesizer for synthesizing a plurality of compounds simultaneously.

【0002】[0002]

【従来の技術】製薬、ライフサイエンス、化学、材料等
の研究分野では、複数の化合物を試験的に同時合成し、
合成物の特性や合成条件等の測定を行う場合があり、こ
のような複数の化合物の同時合成を行う合成機が知られ
ている。
2. Description of the Related Art In research fields such as pharmaceuticals, life sciences, chemistry, and materials, a plurality of compounds are synthesized simultaneously on a trial basis.
In some cases, the properties of the synthesized product, the synthesis conditions, and the like are measured, and a synthesizer that simultaneously synthesizes a plurality of such compounds is known.

【0003】従来の合成器は、同時合成のための複数の
反応室を備えており、個々の反応室は集合して一体とな
り、反応容器を形成している。この反応容器は、反応室
を外部雰囲気から遮断し、かつ、ろ過ができる機能を備
えている。
[0003] A conventional synthesizer has a plurality of reaction chambers for simultaneous synthesis, and the individual reaction chambers are collectively integrated to form a reaction vessel. This reaction vessel has a function of shutting off the reaction chamber from the external atmosphere and performing filtration.

【0004】さらに、ヒータや冷却装置で温度制御され
た部品を押し付けることにより、反応室を所望の温度に
制御できる。
Further, the temperature of the reaction chamber can be controlled to a desired temperature by pressing a component whose temperature is controlled by a heater or a cooling device.

【0005】[0005]

【発明が解決しようとする課題】従来の合成機の反応部
は、複数の反応室が一つの反応容器に一体に形成された
構成であるため、個々の反応室を切り離すことができ
ず、反応室に一つでも破損や汚染が発生した場合には、
反応容器全体をブロックごと交換しなけらばならず、反
応容器にむだが発生するという問題点がある。
The reaction section of the conventional synthesizer has a structure in which a plurality of reaction chambers are integrally formed in one reaction vessel. If any of the rooms are damaged or contaminated,
There is a problem in that the entire reaction vessel must be replaced for each block, and waste occurs in the reaction vessel.

【0006】また、反応容器の温度制御を、反応容器に
伝熱材料を介して密着させた反応温度制御ブロックによ
って行う構成であるため、反応温度制御ブロック内に設
けたヒータや熱媒流路と反応容器の間の距離が長くなっ
たり、反応温度制御ブロックと反応容器との間の接触不
良によって熱伝導効率が低下し、良好な温度制御の制御
特性が得られにくいという問題点がある。
Further, since the temperature of the reaction vessel is controlled by a reaction temperature control block which is brought into close contact with the reaction vessel via a heat transfer material, a heater and a heat medium passage provided in the reaction temperature control block are provided. There is a problem in that the distance between the reaction vessels becomes long, or the heat conduction efficiency is reduced due to poor contact between the reaction temperature control block and the reaction vessel, and it is difficult to obtain good temperature control characteristics.

【0007】さらに、反応容器は複数の反応室のみを一
体に形成した構成であるため、反応室内に試薬と共に注
入された溶媒は加熱によって気化されて蒸発する場合が
あるため、十分な反応を行うことができないという問題
点もある。
Further, since the reaction vessel has a structure in which only a plurality of reaction chambers are integrally formed, the solvent injected together with the reagents into the reaction chamber may be vaporized and evaporated by heating, so that a sufficient reaction is performed. There is also a problem that it is not possible.

【0008】そこで、本発明は前記した従来の合成機の
持つ問題点を解決し、反応容器の交換時のむだを減少さ
せることを第1の目的とし、反応容器の温度制御の制御
特性を向上させることを第2の目的とし、容易に洗浄を
行うことができる反応容器を提供することを第3の目的
とし、又、反応容器中の溶媒の蒸発を減少させることを
第4の目的とする。
Accordingly, the present invention has as its first object to solve the above-mentioned problems of the conventional synthesizing machine and to reduce the uselessness at the time of replacing the reaction vessel, and to improve the control characteristics of the temperature control of the reaction vessel. The second object is to provide a reaction vessel that can be easily washed, and the fourth object is to reduce evaporation of a solvent in the reaction vessel. .

【0009】[0009]

【課題を解決するための手段】本発明の自動合成機は、
その反応部において、化学反応によって複数の化合物の
同時合成を行う複数の反応容器を、各反応容器を個々に
着脱可能に収納する反応ブロックによってブロック化す
ることによって、従来の合成機の持つ問題点を解決する
ものである。
The automatic synthesizer of the present invention comprises:
In the reaction section, a problem with the conventional synthesizer is achieved by blocking a plurality of reaction vessels for simultaneously synthesizing a plurality of compounds by a chemical reaction with reaction blocks that individually and detachably accommodate each reaction vessel. Is to solve.

【0010】本発明の反応ブロックは、例えば、温度,
圧力,振とう,周囲雰囲気等の反応条件を制御し、反応
ブロック内に収納した複数個の反応容器を同一反応条件
とし、複数の化合物の同時合成を行うことができる。
The reaction block of the present invention comprises, for example, temperature,
By controlling reaction conditions such as pressure, shaking, and ambient atmosphere, a plurality of reaction vessels housed in a reaction block can be set to the same reaction conditions to simultaneously synthesize a plurality of compounds.

【0011】本出願の第1の発明は、化学反応により複
数の化合物の同時合成を可能とする自動合成機におい
て、複数個の反応容器と、反応容器を個々に着脱可能と
する収納部を有する反応ブロックを備え、反応ブロック
によって収納部内に収納した反応容器の反応条件の制御
を行う構成とするものであり、これによって、反応容器
の交換時のむだを減少させる第1の目的を達成するもの
である。
A first aspect of the present invention is directed to an automatic synthesizer capable of simultaneously synthesizing a plurality of compounds by a chemical reaction, comprising a plurality of reaction vessels and a storage section for individually detachably attaching the reaction vessels. A reaction block is provided, wherein the reaction block controls the reaction conditions of the reaction container housed in the storage section, thereby achieving the first object of reducing waste when replacing the reaction container. It is.

【0012】第1の発明によれば、複数個の反応容器
は、反応ブロックに形成した収納部に個々に着脱可能で
あるため、収納された反応容器の反応条件を一つの反応
ブロックによって同時に制御することができる。又、破
損や汚染が発生した場合には、該反応容器のみを反応ブ
ロックから取り外し、正常な反応容器に交換することが
できる。これによって、従来の自動合成機のように、全
反応容器を反応ブロックごと交換する必要が無く、反応
容器の交換時のむだを減少させることができる。
According to the first aspect, the plurality of reaction vessels can be individually attached to and detached from the storage section formed in the reaction block, so that the reaction conditions of the stored reaction vessels are simultaneously controlled by one reaction block. can do. Further, when damage or contamination occurs, only the reaction container can be removed from the reaction block and replaced with a normal reaction container. As a result, unlike the conventional automatic synthesizer, it is not necessary to replace all the reaction vessels together with the reaction blocks, and it is possible to reduce waste when replacing the reaction vessels.

【0013】本出願の第2の発明は、化学反応により複
数の化合物の同時合成を可能とする自動合成機におい
て、複数個の反応容器と、反応容器を個々に着脱可能と
する収納部と熱交換手段を伝熱部材内に有した反応ブロ
ックとを備え、熱交換手段によって、収納部内に収納し
た反応容器の温度条件の制御を行う構成とするものであ
り、これによって、反応容器の温度制御の制御特性を向
上させる第2の目的、及び、容易に洗浄を行うことがで
きる反応容器を提供する第3の目的を達成するものであ
る。
A second invention of the present application is directed to an automatic synthesizer capable of simultaneously synthesizing a plurality of compounds by a chemical reaction, comprising a plurality of reaction vessels, a storage section for individually detachable reaction vessels, and a heat storage section. A reaction block having an exchange means in the heat transfer member, wherein the heat exchange means controls the temperature condition of the reaction vessel stored in the storage section, whereby the temperature control of the reaction vessel is performed. The second object of the present invention is to achieve the second object of improving the control characteristics of the present invention and the third object of providing a reaction vessel that can be easily washed.

【0014】第2の発明によれば、反応ブロック内に反
応温度の制御を行う熱交換手段を設け、該反応ブロック
を伝熱部材で形成する構成であるため、熱交換手段と反
応容器との距離が短くなり、又、反応容器と反応温度制
御ブロックとの間に入れた伝熱材料との接触による熱伝
導を行わないため熱伝導効率が高まり、反応容器の温度
制御の制御特性を向上させることができる。
According to the second aspect of the present invention, the heat exchange means for controlling the reaction temperature is provided in the reaction block, and the reaction block is formed by the heat transfer member. The distance is shortened, and heat conduction is not performed by contact with a heat transfer material inserted between the reaction vessel and the reaction temperature control block, so that heat conduction efficiency is increased, and control characteristics of temperature control of the reaction vessel are improved. be able to.

【0015】又、第2の発明によれば、内蔵した熱交換
手段により反応ブロックに反応温度制御の機能を持たせ
ることによって、反応温度制御ブロックを不要とした構
成とし、又、反応容器を反応ブロックに対して着脱可能
な構成とすることによって、反応容器に付着する物質の
洗浄を容易とすることができる。
According to the second aspect of the present invention, the reaction block is provided with a function of controlling the reaction temperature by the built-in heat exchange means, thereby eliminating the need for the reaction temperature control block. By adopting a structure that can be attached to and detached from the block, it is possible to easily clean a substance attached to the reaction container.

【0016】本出願の第3の発明は、化学反応により複
数の化合物の同時合成を可能とする自動合成機におい
て、複数個の反応容器と、反応容器を個々に着脱可能と
する収納部と熱交換手段を伝熱部材内に有した反応ブロ
ックと、反応容器に対応した複数の還流容器を着脱可能
に有する還流ブロックとを備え、反応容器内の気化物質
を還流容器内で凝縮させる構成とするものであり、これ
によって、反応容器中の溶媒の蒸発を減少させる第4の
目的を達成するものである。
According to a third aspect of the present invention, there is provided an automatic synthesizer capable of simultaneously synthesizing a plurality of compounds by a chemical reaction, comprising: a plurality of reaction vessels; It is provided with a reaction block having exchange means in the heat transfer member, and a reflux block having a plurality of detachable reflux containers corresponding to the reaction containers so that vaporized substances in the reaction container are condensed in the reflux container. This achieves the fourth object of reducing the evaporation of the solvent in the reaction vessel.

【0017】第3の発明によれば、反応容器に対応して
複数の還流容器を着脱可能に有する還流ブロックを設け
ることによって、反応容器で気化した溶媒等の成分を凝
縮させて液化させ、再び反応容器に戻すことができ、反
応容器中の溶媒の蒸発による減少を防ぐことができる。
According to the third aspect of the invention, by providing a reflux block having a plurality of detachable reflux vessels corresponding to the reaction vessel, components such as a solvent vaporized in the reaction vessel are condensed and liquefied, and are again liquefied. It can be returned to the reaction vessel, and a decrease due to evaporation of the solvent in the reaction vessel can be prevented.

【0018】本出願の第4の発明は、第1〜3の発明に
おいて、反応容器は、反応室と、化合物を導出する導出
管及び導出部と、反応室の下方側と導出管の上方側とを
接続する接続管とを備え、反応室と導出管は並列して配
置し、接続管は反応室と導出管が形成する面に対して傾
斜して配置する構成とするものであり、これによって第
1〜4の目的を達成すると共に、反応室,接続管,及び
導出管の径を拡張することができる。
According to a fourth aspect of the present invention, in the first to third aspects, the reaction vessel comprises a reaction chamber, an outlet pipe and an outlet for discharging the compound, a lower side of the reaction chamber and an upper side of the outlet pipe. And a connecting pipe for connecting the reaction chamber and the outlet pipe, and the connecting pipe is arranged to be inclined with respect to a surface formed by the reaction chamber and the outlet pipe. Thus, the first to fourth objects can be achieved, and the diameters of the reaction chamber, the connecting pipe, and the outlet pipe can be expanded.

【0019】第4の発明によれば、反応室と導出管とが
形成する面からずれた位置に接続管を配置することによ
って、反応容器内において導出管と反応室とに干渉しな
い空間に接続管を形成することができ、反応容器の外形
寸法に制限がある場合であっても、反応室,接続管,及
び導出管の径を拡張することができる。
According to the fourth aspect of the present invention, the connection pipe is disposed at a position deviated from the plane formed by the reaction chamber and the outlet pipe, so that the connection pipe is connected to a space in the reaction vessel that does not interfere with the outlet pipe and the reaction chamber. A tube can be formed, and the diameter of the reaction chamber, the connecting tube, and the outlet tube can be expanded even when the external dimensions of the reaction vessel are limited.

【0020】反応室の径を拡張することによって、化合
物を生成する反応空間の容積を拡大して生成物の生成量
を増加させることができ、接続管の径を拡張することに
よって、反応室と導出管との間を接続する通路部分の目
詰まりを防止することができる。また、導出管の径を拡
張することによって、接続管を介して反応室から導出さ
れた生成物の液切れを良好なものとすることができる。
By expanding the diameter of the reaction chamber, it is possible to increase the volume of the product by increasing the volume of the reaction space for producing the compound. It is possible to prevent clogging of a passage portion connecting to the outlet pipe. In addition, by expanding the diameter of the outlet pipe, it is possible to make the liquid discharged from the reaction chamber through the connection pipe drain better.

【0021】本出願の第5の発明は、第1〜4の発明に
おいて、反応容器を収納するブロックに複数個の凹部を
設け、凹部の底面の一部に反応容器を挿入する開口部を
設け、凹部をブロック上面に形成されるガス供給用溝に
より連結する構成とするものであり、これによって第1
〜4の目的を達成すると共に、反応容器から溢れた生成
物が飛散して他の反応容器を汚染することを防止するこ
とができる。
According to a fifth aspect of the present invention, in the first to fourth aspects, a plurality of recesses are provided in a block for accommodating the reaction vessel, and an opening for inserting the reaction vessel is provided in a part of the bottom surface of the recess. , The recesses are connected by a gas supply groove formed on the upper surface of the block.
In addition to achieving the objects of (1) to (4), it is possible to prevent products overflowing from the reaction vessel from scattering and contaminating other reaction vessels.

【0022】ガス供給用溝を介して各反応容器内に窒素
やアルゴン等の不活性ガスを供給し、ガス圧力によって
反応容器内に設置したフィルターを通して生成物のろ過
を行い、反応容器内の液体成分の導出を行う。
An inert gas such as nitrogen or argon is supplied into each reaction vessel through the gas supply groove, and the product is filtered through a filter installed in the reaction vessel by gas pressure, and the liquid in the reaction vessel is supplied. Derivation of components.

【0023】第5の発明によれば、反応容器はブロック
に形成した凹部に形成した開口部内に挿入され、各凹部
はガス供給用溝で連結されているため、反応容器から溢
れた生成物は凹部に溜まって、他の反応容器への流出を
防止することができる。また、他の反応容器に流出した
場合であっても、該反応容器の凹部によって生成物の流
速が低下して凹部面上に沈下し、下流の反応容器への飛
散を防止することができる。
According to the fifth invention, the reaction vessel is inserted into the opening formed in the recess formed in the block, and each recess is connected by the gas supply groove. Accumulation in the concave portion prevents outflow to another reaction vessel. Further, even when the product flows out to another reaction vessel, the flow rate of the product is reduced by the concave portion of the reaction container and sinks on the surface of the concave portion, so that it is possible to prevent the product from scattering to the downstream reaction container.

【0024】本発明の実施の態様によれば、熱交換手段
は、熱媒流路およびヒーターとすることができ、反応ブ
ロックには熱媒流路およびヒーターを設け、還流ブロッ
クには熱媒流路を設けることができる。本発明の実施の
態様によれば、反応容器はフィルターを備え、さらに、
フィルターを介して外部と通じる導出管は保守用押しね
じを備える。
According to the embodiment of the present invention, the heat exchange means can be a heat medium flow path and a heater, the reaction block is provided with a heat medium flow path and a heater, and the reflux block is provided with a heat medium flow path and a heater. Roads can be provided. According to an embodiment of the present invention, the reaction vessel includes a filter, further comprising:
The outlet pipe communicating with the outside through the filter is provided with a maintenance screw.

【0025】[0025]

【発明の実施の形態】以下、本発明の実施の形態を図を
参照しながら詳細に説明する。図1は、本発明の反応容
器及び還流容器の概略を説明するための断面図であり、
図2,3,4は本発明の自動合成機反応部の概略を説明
するための一部を切り欠いた斜視図であり、図2は反応
ブロックと還流ブロックを組み合わせた状態を示し、図
3は還流ブロックを示し、図4は反応ブロックを示して
いる。図5,6は図2に示す自動合成機反応部の断面図
であり、図2中に示す方向A,Bから見た断面を示して
いる。又、図7は還流ブロックの上面、及び反応ブロッ
クないし還流ブロック内の熱交換手段の配置を示す平面
図である。
Embodiments of the present invention will be described below in detail with reference to the drawings. FIG. 1 is a cross-sectional view schematically illustrating a reaction vessel and a reflux vessel of the present invention,
FIGS. 2, 3, and 4 are partially cutaway perspective views for explaining the outline of the reaction section of the automatic synthesizer of the present invention, and FIG. 2 shows a state where a reaction block and a reflux block are combined. Shows a reflux block, and FIG. 4 shows a reaction block. FIGS. 5 and 6 are cross-sectional views of the reaction section of the automatic synthesizer shown in FIG. 2, and show cross sections viewed from directions A and B shown in FIG. FIG. 7 is a plan view showing the upper surface of the reflux block and the arrangement of the heat exchange means in the reaction block or the reflux block.

【0026】本発明の自動合成機は、その反応部1にお
いて、図1に示すような反応容器3及び還流容器2を複
数個備え、各反応容器3内に試薬や溶媒等の合成に必要
な物質を注入し、温度,圧力,振とう,周囲雰囲気等の
条件制御下で反応およびろ過して、化合物の合成を行
う。反応容器3は、合成に必要な物質を注入し化合物の
合成を行う反応室31と、フィルター35でろ過したろ
過物質を外部に取り出す導出管32及び導出部33と、
導出管32等の細管のつまりを除くための保守用押しね
じ34を備える。又、還流容器2は、反応容器3内で気
化した物質を凝縮させて液化させるための容器であっ
て、反応容器3の上方に取り付けられ、反応容器3内へ
の物質の注入を行うための開口部21と、気密性を保持
するためのOリング等のパッキング22を備える。な
お、反応容器3及び還流容器2はテフロン,ポリプロピ
レン等の合成樹脂で形成することができる。テフロンを
用いた場合には化学反応に対する耐性が良く、ポリプロ
ピレンを用いた場合には安価で形成することができ、使
い捨てが容易となる。
The automatic synthesizer of the present invention includes a plurality of reaction vessels 3 and a plurality of reflux vessels 2 as shown in FIG. The compound is synthesized by injecting the substance, reacting and filtering under conditions such as temperature, pressure, shaking, and ambient atmosphere. The reaction vessel 3 includes a reaction chamber 31 for injecting a substance necessary for the synthesis and synthesizing the compound, an outlet pipe 32 and an outlet 33 for taking out the filtered substance filtered by the filter 35 to the outside,
A maintenance push screw 34 for removing the clogging of a thin tube such as the outlet tube 32 is provided. The reflux vessel 2 is a vessel for condensing and liquefying a substance vaporized in the reaction vessel 3, and is mounted above the reaction vessel 3 and used for injecting the substance into the reaction vessel 3. An opening 21 and a packing 22 such as an O-ring for maintaining airtightness are provided. The reaction vessel 3 and the reflux vessel 2 can be formed of a synthetic resin such as Teflon or polypropylene. When Teflon is used, it has good resistance to a chemical reaction, and when polypropylene is used, it can be formed at a low cost and can be easily disposable.

【0027】図2,5,6において、自動合成機反応部
1は還流ブロック4と反応ブロック5を備える。還流ブ
ロック4は、図2,3に示すように、アルミニウム等で
形成される伝熱部材を兼ねた還流ブロック本体41と、
還流ブロック本体41の下面に取り付けられて、熱媒流
路48を保持する熱媒流路押さえ42とを有している。
熱媒流路押さえ42は断熱材を兼ねることができ、テフ
ロンで形成することができる。
In FIGS. 2, 5 and 6, the automatic synthesizer reaction section 1 includes a reflux block 4 and a reaction block 5. The reflux block 4 includes, as shown in FIGS. 2 and 3, a reflux block main body 41 formed of aluminum or the like and also serving as a heat transfer member.
It has a heat medium flow channel holder 42 that is attached to the lower surface of the reflux block main body 41 and holds the heat medium flow channel 48.
The heat medium flow channel retainer 42 can also serve as a heat insulating material, and can be formed of Teflon.

【0028】還流ブロック本体41には複数個の還流容
器2を収納する複数の収納部43が形成され、上面には
反応容器3内に試薬や溶媒等の合成に必要な物質を注入
するための開口部が形成され、又、熱媒流路押さえ42
には還流容器2のフランジ部分やパッキング22を収納
する凹部が形成される。又、還流ブロック本体41内に
は、図7(b)に示すように、熱媒流路48を収納部4
3と交差しないよう配置する。熱媒流路48中に熱媒を
流すことによって、還流ブロック本体41を伝熱部材と
して、収納部43内に収納した還流容器2の温度制御を
行う。例えば、熱媒の温度が0℃であれば、熱媒流路4
8と接触している還流ブロック本体41を介して還流容
器2も熱媒に近い温度に冷却される。
A plurality of storage portions 43 for storing a plurality of reflux containers 2 are formed in the reflux block main body 41. On the upper surface, a substance necessary for synthesizing a reagent, a solvent or the like necessary for synthesis into the reaction container 3 is provided. An opening is formed.
Is formed with a flange portion of the reflux container 2 and a concave portion for accommodating the packing 22. In addition, as shown in FIG. 7B, a heat medium flow path 48 is provided in the storage block 4 in the reflux block main body 41.
3 so that they do not intersect. By flowing the heat medium through the heat medium flow path 48, the temperature of the reflux container 2 housed in the housing part 43 is controlled using the reflux block main body 41 as a heat transfer member. For example, if the temperature of the heat medium is 0 ° C., the heat medium flow path 4
The reflux vessel 2 is also cooled to a temperature close to the heat medium via the reflux block main body 41 that is in contact with 8.

【0029】還流ブロック本体41に対する還流容器2
の脱着は、熱媒流路押さえ42に形成された開口部を通
して行い、還流容器2のフランジ部を還流ブロック本体
41及び熱媒流路押さえ42ではさみ、図示しない固定
具で固定することによって還流容器2の所定位置への固
定を行うことができる。
The reflux container 2 with respect to the reflux block main body 41
Is carried out through an opening formed in the heat medium flow channel holder 42, the flange portion of the reflux container 2 is sandwiched between the reflux block main body 41 and the heat medium flow channel holder 42, and fixed by a fixture (not shown). The container 2 can be fixed at a predetermined position.

【0030】還流ブロック4の上面には、テフロン、フ
ッ素ゴム等で形成されるシール材6をはさんでアルミニ
ウム等で形成される上蓋7が取り付けられる。還流ブロ
ック4の上面とシール材6との間の密着性を高めて外気
との遮断を行うために、還流ブロック4の上面に溝45
を形成し、該溝45内にシール材6に形成した凸部61
を押し込む構成とすることができる。
An upper lid 7 made of aluminum or the like is attached to the upper surface of the reflux block 4 with a sealing material 6 made of Teflon, fluoro rubber or the like interposed therebetween. Grooves 45 are formed in the upper surface of the reflux block 4 in order to increase the adhesion between the upper surface of the reflux block 4 and the sealing material 6 to block the outside air.
Formed in the groove 45, and a convex portion 61 formed in the sealing material 6 in the groove 45.
Can be pressed.

【0031】又、還流ブロック4の上面の収納部43に
隣接してガス用溝44を形成し、このガス用溝44を通
して反応容器3内に窒素やアルゴン等の不活性ガスを供
給し、その圧力によってフィルターを通してろ過させ、
反応容器3内の液体成分の排出を行うことができる。な
お、上記ガス用溝44に代えて、シール材6に円筒形の
ニードルを突き刺し、不活性ガスを供給する構成とする
こともできる。この構成によれば、反応容器の内容物を
個別にろ過することができる。
A gas groove 44 is formed adjacent to the storage section 43 on the upper surface of the reflux block 4, and an inert gas such as nitrogen or argon is supplied into the reaction vessel 3 through the gas groove 44. Filtered through a filter by pressure,
The liquid component in the reaction vessel 3 can be discharged. Note that, instead of the gas groove 44, a cylindrical needle may be inserted into the sealing material 6 to supply an inert gas. According to this configuration, the contents of the reaction vessel can be individually filtered.

【0032】又、上蓋7には、還流容器2及び反応容器
3に通じる開口部71が形成され、該開口部71を通し
て上記ニードル等をシール材6に貫通させ、反応容器3
内に試薬や溶媒等の合成に必要な物質の注入や不活性ガ
スの供給を行うことができる。
The upper lid 7 is formed with an opening 71 communicating with the reflux vessel 2 and the reaction vessel 3.
A substance necessary for the synthesis of a reagent, a solvent, or the like can be injected into the inside, or an inert gas can be supplied.

【0033】反応ブロック5は、図2,4に示すよう
に、アルミニウム等で形成される伝熱部材を兼ねた反応
ブロック本体51と、反応ブロック本体51の上面に取
り付けられて、熱媒流路58を保持する熱媒流路押さえ
54と、反応ブロック本体51の下面に取り付けられ
て、ヒータ59を保持するヒータ押さえ52とを有して
いる。両押さえ52,54は断熱材を兼ねることがで
き、テフロンで形成することができる。
The reaction block 5 is, as shown in FIGS. 2 and 4, a reaction block main body 51 made of aluminum or the like and also serving as a heat transfer member. It has a heat medium flow channel holder 54 for holding 58, and a heater holder 52 attached to the lower surface of the reaction block main body 51 and holding a heater 59. Both retainers 52 and 54 can also serve as a heat insulating material, and can be formed of Teflon.

【0034】反応ブロック本体51には複数個の反応容
器3を収納する複数の収納部53が形成され、熱媒流路
押さえ54には反応容器3を挿入し、上端部分を突出さ
せるための開口部が形成され、ヒータ押さえ52には反
応容器3の導出部33を外部に通すための開口部55が
形成される。反応ブロック本体51に対する反応容器3
の脱着は、熱媒流路押さえ54に形成された開口部を通
して行い、反応容器3の底部をヒータ押さえ52に当接
させることによって反応容器3の位置決めを行うことが
できる。
A plurality of storage sections 53 for storing a plurality of reaction vessels 3 are formed in the reaction block main body 51, and an opening for inserting the reaction vessel 3 into the heat medium channel holder 54 and projecting an upper end portion thereof. An opening 55 is formed in the heater retainer 52 to allow the outlet 33 of the reaction vessel 3 to pass outside. Reaction vessel 3 for reaction block body 51
The reaction vessel 3 can be positioned by bringing the bottom of the reaction vessel 3 into contact with the heater retainer 52 through the opening formed in the heat medium flow path retainer 54.

【0035】又、反応ブロック本体51内には、熱媒流
路58及びヒータ59が配置される。図7(b)は反応
ブロック本体51内の熱媒流路58及びヒータ59の配
置を示す図であり、熱媒流路58及びヒータ59を収納
部53と交差しないよう配置する。熱媒流路58中に熱
媒を流すことによって、反応ブロック本体51を伝熱部
材として収納部53内に収納した反応容器3を冷却また
は加熱する。又、ヒータ59を駆動することによって、
反応ブロック本体51を伝熱部材として収納部53内に
収納した反応容器3を加熱する。
In the reaction block main body 51, a heating medium passage 58 and a heater 59 are arranged. FIG. 7B is a diagram showing the arrangement of the heat medium flow path 58 and the heater 59 in the reaction block main body 51. The heat medium flow path 58 and the heater 59 are arranged so as not to intersect with the storage section 53. By flowing a heat medium into the heat medium flow path 58, the reaction container 3 housed in the housing 53 with the reaction block body 51 as a heat transfer member is cooled or heated. Also, by driving the heater 59,
The reaction vessel 3 housed in the housing 53 with the reaction block body 51 as a heat transfer member is heated.

【0036】例えば、熱媒の温度が60℃であれば、熱
媒流路58と接触している反応ブロック本体51を介し
て反応容器3も熱媒に近い温度に加熱される。また、ヒ
ータ59によってさらに高温に加熱することができ、温
度制御は図示しない温度センサとコントローラにより行
うことができ、定温に保持することもできる。
For example, if the temperature of the heat medium is 60 ° C., the reaction vessel 3 is also heated to a temperature close to the heat medium via the reaction block main body 51 in contact with the heat medium flow path 58. The temperature can be further increased by the heater 59, the temperature can be controlled by a temperature sensor and a controller (not shown), and the temperature can be maintained at a constant value.

【0037】本発明の自動合成機の反応部は、反応容器
を着脱自在とする反応ブロックのみを備え、前記還流ブ
ロックを省いた構成とすることもできる。図8は本発明
の自動合成機の反応部の他の構成を説明するための図で
ある。図8において、自動合成機の反応部は反応ブロッ
ク本体51の上下端にヒータ押さえ52と熱媒流路押さ
え54を備えた反応ブロック5により構成される。熱媒
流路押さえ54には収納部53’が形成され、反応ブロ
ック本体51に形成される収納部53と連通して反応容
器3を収納する。なお、図8には図示していないが、熱
媒流路押さえ54の上方には、図2,3と同様に、シー
ル材6をはさんで上蓋7が取り付けられる。
The reaction section of the automatic synthesizer according to the present invention may be provided with only a reaction block in which a reaction container is detachable, and the reflux block may be omitted. FIG. 8 is a view for explaining another configuration of the reaction section of the automatic synthesizer of the present invention. In FIG. 8, the reaction section of the automatic synthesizer includes a reaction block 5 having a heater holder 52 and a heat medium passage holder 54 at the upper and lower ends of a reaction block main body 51. A storage section 53 ′ is formed in the heat medium flow channel holder 54, and stores the reaction container 3 in communication with the storage section 53 formed in the reaction block main body 51. Although not shown in FIG. 8, an upper lid 7 is attached above the heat medium flow channel retainer 54 with the sealing material 6 interposed therebetween as in FIGS. 2 and 3.

【0038】本発明の自動合成機の反応容器の他の構成
を図9、図10を用いて説明する。なお、図9(a)は
反応容器を上方から見た平面図であり、図9(b)は反
応容器の径方向(図9(a)中のA−A)の断面図であ
り、図9(c)は図9(a)中のB−Bで示す断面図で
ある。また、図10は反応容器の内部空間を示す透視図
である。
Another configuration of the reaction vessel of the automatic synthesizer of the present invention will be described with reference to FIGS. 9 (a) is a plan view of the reaction vessel viewed from above, and FIG. 9 (b) is a sectional view of the reaction vessel in a radial direction (AA in FIG. 9 (a)). FIG. 9C is a cross-sectional view taken along line BB in FIG. 9A. FIG. 10 is a perspective view showing the internal space of the reaction vessel.

【0039】図9,10に示す反応容器3は、図1で示
した構成と同様に、合成に必要な物質を注入し化合物の
合成を行う反応室31と、フィルター(図示していな
い)でろ過した生成物のろ過物質を外部に取り出す導出
管32及び導出部33と、反応室31の下方側と導出管
36の上方側とを接続する接続管36と、導出管32や
接続管36の細管のつまりを除くための保守用押しねじ
34を備え、接続管36は反応室31と導出管32とが
形成する面に対して傾斜して配置する。
The reaction vessel 3 shown in FIGS. 9 and 10 has a reaction chamber 31 for injecting a substance necessary for synthesis and synthesizing a compound, and a filter (not shown), as in the configuration shown in FIG. An outlet pipe 32 and an outlet 33 for taking out the filtered substance of the filtered product to the outside, a connecting pipe 36 connecting the lower side of the reaction chamber 31 and the upper side of the outlet pipe 36, and a connecting pipe 36 of the connecting pipe 36. A maintenance push screw 34 for removing the clogging of the thin tube is provided, and the connecting tube 36 is arranged to be inclined with respect to the surface formed by the reaction chamber 31 and the outlet tube 32.

【0040】接続管36を反応室31と導出管32とが
形成する面に対する傾斜配置は、反応室31と導出管3
2とを反応容器3の直径線上(図9(a)のA−A)に
配列すると共に、反応室31の下端部分に反応室31の
底面から横方向に突出した空間部分37を形成し、接続
管36の上端を該直径線(図9(a)のA−A)からず
れた位置で導出管32の上端と接続し、接続管36の下
端を横方向に突出した空間部分37に接続することによ
って構成することができる。空間部分37は図9,10
に示す形状に限るものではなく、接続管36を反応容器
3内で傾斜させる任意の形状とすることができる。
The connecting pipe 36 is inclined with respect to the plane formed by the reaction chamber 31 and the outlet pipe 32.
2 are arranged on the diameter line of the reaction vessel 3 (A-A in FIG. 9A), and a space portion 37 is formed at the lower end of the reaction chamber 31 so as to project laterally from the bottom surface of the reaction chamber 31. The upper end of the connecting pipe 36 is connected to the upper end of the lead-out pipe 32 at a position shifted from the diameter line (A-A in FIG. 9A), and the lower end of the connecting pipe 36 is connected to the space 37 protruding in the lateral direction. Can be configured. The space 37 is shown in FIGS.
The connection pipe 36 is not limited to the shape shown in FIG.

【0041】なお、図9,10において、接続管36の
上端と導出管32の上端は、保守用押しねじ34が収納
される凹部で接続されている。
In FIGS. 9 and 10, the upper end of the connecting pipe 36 and the upper end of the outlet pipe 32 are connected by a recess in which the maintenance push screw 34 is stored.

【0042】図9(b),(c)、及び図10に示すよ
うに、接続管36は反応容器3内の空間において反応室
31と導出管32とが形成する空間の隙間部分に配設さ
れる。この配置によって、反応室31,接続管36,及
び導出管32を反応容器3の直径線上に配列した場合と
比較して、各室及び管の径を拡張することができる。
As shown in FIGS. 9 (b), 9 (c) and 10, the connecting pipe 36 is disposed in the space inside the reaction vessel 3 in the space defined by the reaction chamber 31 and the outlet pipe 32. Is done. With this arrangement, the diameter of each chamber and tube can be expanded as compared with the case where the reaction chamber 31, the connection pipe 36, and the outlet pipe 32 are arranged on the diameter line of the reaction vessel 3.

【0043】次に、本発明の自動合成機の反応容器にガ
スを供給する溝の他の構成を図11を用いて説明する。
ガス供給用溝44は、前記したように、各反応容器3内
に窒素やアルゴン等の不活性ガスを供給し、ガス圧力に
よって反応容器3内に設置したフィルターを通して生成
物のろ過を行い、反応容器3内の生成物の液体成分の導
出を行う。
Next, another configuration of the groove for supplying gas to the reaction vessel of the automatic synthesizer of the present invention will be described with reference to FIG.
As described above, the gas supply groove 44 supplies an inert gas such as nitrogen or argon into each of the reaction vessels 3 and filters a product through a filter provided in the reaction vessel 3 by gas pressure. The liquid component of the product in the container 3 is derived.

【0044】図11は、反応ブロック本体5の上面にガ
ス供給用溝44を形成した場合について示している。反
応ブロック本体5の熱媒流路押さえ54には収納部5
3’が形成され、反応ブロック本体51に形成される収
納部53と連通して反応容器3を収納する。また、図示
していないが熱媒流路押さえ54の上方には、シール材
6をはさんで上蓋7が取り付けられる。
FIG. 11 shows a case where a gas supply groove 44 is formed on the upper surface of the reaction block main body 5. The heating medium channel holder 54 of the reaction block main body 5 has a housing 5
A reaction vessel 3 is formed in communication with a storage section 53 formed in the reaction block main body 51. Although not shown, an upper lid 7 is attached above the heat medium flow channel retainer 54 with the sealing material 6 interposed therebetween.

【0045】熱媒流路押さえ54の上面において、収納
部53’が形成される部分には凹部46が形成される。
凹部46の底面の一部に開口部を形成し、該開口部を収
納部53’の上端部とする。凹部46は、熱媒流路押さ
え54の上面に収納部53’に対応して複数個設けられ
る。各凹部46は、熱媒流路押さえ54の上面に形成さ
れたガス供給用溝44によって連結される。
On the upper surface of the heat medium flow channel holder 54, a concave portion 46 is formed at a portion where the storage portion 53 'is formed.
An opening is formed in a part of the bottom surface of the concave portion 46, and the opening is used as the upper end of the storage portion 53 '. A plurality of concave portions 46 are provided on the upper surface of the heat medium flow channel retainer 54 in correspondence with the storage portions 53 '. Each of the concave portions 46 is connected by a gas supply groove 44 formed on the upper surface of the heat medium flow channel retainer 54.

【0046】凹部46の底面部分の面積は、収納部5
3’内に収納される反応室3の上端面の面積よりも十分
に広く形成される。反応室3の生成物がオーバーフロー
した場合、溢れた生成物はこの凹部46の底面に溜ま
り、ガス供給用溝44を介して他の反応室3に流れるこ
とを防止する。また、生成物がガス供給用溝44を介し
て他の凹部46に流れ込む場合であっても、ガス供給用
溝44から凹部46に流れ込む際に流速が大幅に低下
し、さらに他の凹部にの流れ込むことを防止する。
The area of the bottom surface of the concave portion 46 is
It is formed sufficiently wider than the area of the upper end face of the reaction chamber 3 housed in 3 ′. When the product in the reaction chamber 3 overflows, the overflowed product accumulates on the bottom surface of the concave portion 46 to prevent the product from flowing into another reaction chamber 3 through the gas supply groove 44. Further, even when the product flows into the other concave portion 46 through the gas supply groove 44, the flow velocity is significantly reduced when flowing into the concave portion 46 from the gas supply groove 44, and further, the flow into the other concave portion is reduced. Prevents inflow.

【0047】なお、前記凹部及びガス供給用溝は、反応
ブロック本体に限らず環流ブロック本体等の反応容器を
収納するブロックに形成することができる。
The concave portion and the gas supply groove can be formed not only in the reaction block main body but also in a block for accommodating a reaction vessel such as a reflux block main body.

【0048】次に、本発明の自動合成機による合成手順
について説明する。収納部53内に反応容器3を収納し
た反応ブロック51と、収納部43内に還流容器3を収
納した還流ブロック41を用意し、反応ブロック51の
熱媒流路押さえ54に上面に還流ブロック4を取り付
け、さらに、還流ブロック41の上面にシール材6及び
上蓋7を取り付け、固定具で固定を行うことにより自動
合成機反応部1の組立を行う。
Next, the synthesis procedure by the automatic synthesizer of the present invention will be described. A reaction block 51 containing the reaction vessel 3 in the storage section 53 and a reflux block 41 containing the reflux vessel 3 in the storage section 43 are prepared. The sealing member 6 and the upper lid 7 are further attached to the upper surface of the reflux block 41, and are fixed with a fixture to assemble the reaction section 1 of the automatic synthesizer.

【0049】この組立において、反応容器3内に反応に
用いる試薬や溶媒の注入を行う。なお、自動合成機反応
部1の組立の後、上蓋7に形成した開口部71を通して
シール材6にニードルを刺し込み、反応容器3内に反応
に用いる試薬や溶媒の注入を行うこともできる。
In this assembly, reagents and solvents used for the reaction are injected into the reaction vessel 3. After assembling the reaction section 1 of the automatic synthesizer, a needle may be inserted into the sealing material 6 through the opening 71 formed in the upper lid 7 to inject the reagent or solvent used for the reaction into the reaction vessel 3.

【0050】反応ブロック3の熱媒流路58に熱媒を流
したり、ヒータ59を駆動することによって、反応容器
3内の試薬や溶媒を冷却または加熱して、反応条件の温
度制御を行う。また、ガス用溝44から不活性ガスを供
給して圧力制御を行ったり、反応ブロック3全体を振と
うさせることもできる。
By flowing a heat medium through the heat medium flow path 58 of the reaction block 3 or driving the heater 59, the reagent or solvent in the reaction vessel 3 is cooled or heated to control the temperature of the reaction conditions. In addition, an inert gas may be supplied from the gas groove 44 to perform pressure control, or the entire reaction block 3 may be shaken.

【0051】加熱による反応を行わせるとき、溶媒の沸
点が試薬の沸点よりも低い場合には、溶媒成分は試薬よ
り先に気化する。気化した溶媒成分は、反応容器3の上
方に設置された還流容器2に到達する。このとき、還流
ブロック4中の熱媒流路48に冷媒を流して還流容器2
を冷却すると、気化した溶媒成分は冷却されて凝縮し、
液体となって反応容器3内に戻される。これによって、
溶媒が蒸発して消失することを防止することができる。
When the reaction is carried out by heating, if the boiling point of the solvent is lower than the boiling point of the reagent, the solvent component is vaporized before the reagent. The vaporized solvent component reaches the reflux vessel 2 installed above the reaction vessel 3. At this time, the refrigerant flows through the heat medium flow path 48 in the reflux block 4 to
Is cooled, the vaporized solvent component is cooled and condensed,
It is returned to the reaction vessel 3 as a liquid. by this,
The solvent can be prevented from evaporating and disappearing.

【0052】反応の後、合成された物質をろ過する場合
には、図示しないガス源から不活性ガスを導入し、ガス
用溝44を通して反応容器3内に流通させる。反応容器
3の内部は不活性な雰囲気に保たれたまま加圧され、複
数の反応容器3内の液体成分をフィルター35を通して
同時に取り出すことができる。化合物は、ろ過物あるい
は、ろ過残留物として取り出すことができる。
After the reaction, when filtering the synthesized substance, an inert gas is introduced from a gas source (not shown), and is passed through the gas groove 44 into the reaction vessel 3. The inside of the reaction vessel 3 is pressurized while being kept in an inert atmosphere, and the liquid components in the plurality of reaction vessels 3 can be simultaneously taken out through the filters 35. The compound can be taken out as a filtrate or a filtration residue.

【0053】反応容器3の導出管32の細管に穴づまり
が発生した場合には、保守用押しねじ34を外し、細い
棒で導出管32内を清掃することにより穴づまりを解消
することができる。
In the case where the narrow tube of the outlet tube 32 of the reaction vessel 3 is clogged, the clogging of the hole can be eliminated by removing the maintenance push screw 34 and cleaning the inside of the outlet tube 32 with a thin rod.

【0054】又、反応容器3や還流容器2の洗浄を行う
場合には、図示しない固定具を解除して還流ブロック4
と反応ブロック5を分離し、還流ブロック4から還流容
器2を取り外し、反応ブロック5から反応容器3を取り
外して、各還流容器2及び反応容器3を洗浄することが
できる。また、還流ブロック4および反応ブロック5自
体の洗浄を行うこともできる。洗浄した後、再び還流ブ
ロック4内に還流容器2を挿入し、反応ブロック5内に
反応容器3を挿入することによって、自動合成機の反応
部を組み立てることができる。
When the reaction vessel 3 and the reflux vessel 2 are to be washed, the fixture (not shown) is released and the reflux block 4 is removed.
And the reaction block 5, the reflux container 2 is removed from the reflux block 4, the reaction container 3 is removed from the reaction block 5, and the reflux container 2 and the reaction container 3 can be washed. Further, the reflux block 4 and the reaction block 5 can be washed. After the washing, the reaction vessel of the automatic synthesizer can be assembled by inserting the reflux vessel 2 again into the reflux block 4 and inserting the reaction vessel 3 into the reaction block 5.

【0055】前記洗浄と同様の手順によって、破損ある
いは汚染された還流容器あるいは反応容器のみを正常な
容器に交換することができる。なお、自動合成機が備え
る各反応容器は、同一容量とすることも、異なる容量と
することもできる。また、ガス用溝を共有する反応容器
の組み合わせも、任意に行うことができる。
By the same procedure as in the above-described washing, only the damaged or contaminated reflux vessel or reaction vessel can be replaced with a normal vessel. In addition, each reaction container provided in the automatic synthesizer may have the same capacity or different capacities. In addition, a combination of reaction vessels sharing a gas groove can be arbitrarily performed.

【0056】本発明の実施の態様によれば、反応室と導
出管とが形成する面からずれた位置に接続管を配置する
ことによって、反応容器内において導出管と反応室とに
干渉しない空間に接続管を形成することができ、化合物
を生成する反応空間の容積を拡大して生成物の生成量を
増加させ、反応室と導出管との間を接続する接続管の通
路部分の目詰まりを防止することができ、また、導出管
において生成物の液切れを良好なものとすることができ
る。
According to the embodiment of the present invention, by disposing the connecting pipe at a position deviated from the plane formed by the reaction chamber and the outlet pipe, a space that does not interfere with the outlet pipe and the reaction chamber in the reaction vessel is provided. A connection tube can be formed in the reaction space, and the volume of the reaction space for producing the compound is increased to increase the amount of product generated, and the passage portion of the connection tube connecting the reaction chamber and the outlet tube is clogged. Can be prevented, and the product can be desirably drained in the outlet pipe.

【0057】本発明の実施の態様によれば、ブロック面
上に形成した凹部と該凹部を連結するガス供給用溝とに
よって、反応容器から溢れた生成物を凹部に溜め、他の
反応容器への流出を防止することができる。
According to the embodiment of the present invention, the product overflowing from the reaction vessel is stored in the recess by the recess formed on the block surface and the gas supply groove connecting the recess, and is transferred to another reaction vessel. Outflow can be prevented.

【0058】本発明の実施の態様によれば、破損あるい
は汚染された容器のみの交換ができるため、還流ブロッ
クや反応ブロック全体の交換を行う必要が無く、交換費
用を低減させることができる。本発明の実施の態様によ
れば、伝熱ブロックを要さないため、省スペース化、軽
量化を図ることができ、ブロックの振とうが容易とな
る。本発明の実施の態様によれば、ブロック化すること
によって、熱媒流路やヒータ等の熱交換手段の脱着及び
交換が容易となる。
According to the embodiment of the present invention, only the damaged or contaminated vessel can be replaced, so that it is not necessary to replace the entire reflux block or reaction block, and the replacement cost can be reduced. According to the embodiment of the present invention, since no heat transfer block is required, space saving and weight reduction can be achieved, and shaking of the block becomes easy. According to the embodiment of the present invention, the blocking makes it easy to attach and detach heat exchange means such as a heat medium passage and a heater.

【0059】[0059]

【発明の効果】以上説明したように、本発明の自動合成
機によれば、化学反応によって複数の化合物の同時合成
を行う複数の反応容器を、各反応容器を個々に着脱可能
に収納する反応ブロックによってブロック化することに
よって、合成機の持つ問題点を解決することができ、複
数個の反応容器を個々に着脱可能とする収納部を有する
反応ブロックによって収納部内に収納した反応容器の反
応条件の制御を行うことにより、反応容器の交換時のむ
だを減少させることができ、複数個の反応容器を個々に
着脱可能とする収納部と熱交換手段を伝熱部材内に有し
た反応ブロックとを備え、熱交換手段によって収納部内
に収納した反応容器の温度条件の制御を行うことによ
り、反応容器の温度制御の制御特性を向上させ、容易に
洗浄を行うことができ、又、複数個の反応容器を個々に
着脱可能とする収納部と熱交換手段を伝熱部材内に有し
た反応ブロックと、反応容器に対応した複数の還流容器
を着脱可能に有する還流ブロックとを備え、反応容器内
の気化物質を還流容器内で凝縮させる構成とすることに
より、反応容器中の溶媒の蒸発を減少させることができ
る。
As described above, according to the automatic synthesizer of the present invention, a reaction in which a plurality of reaction vessels for simultaneously synthesizing a plurality of compounds by a chemical reaction are detachably accommodated in each reaction vessel. Blocking by the block can solve the problems of the synthesizer, and the reaction conditions of the reaction container stored in the storage unit by the reaction block having the storage unit that allows a plurality of reaction containers to be individually attached and detached. By performing the above control, it is possible to reduce waste when exchanging the reaction vessel, and to provide a reaction block having a storage section and a heat exchange means in the heat transfer member, in which a plurality of reaction vessels can be individually attached and detached. By controlling the temperature condition of the reaction container stored in the storage unit by the heat exchange means, the control characteristics of the temperature control of the reaction container can be improved, and the cleaning can be easily performed. Also, a reaction block having a storage section and a heat exchange means in the heat transfer member, in which a plurality of reaction vessels can be individually attached and detached, and a reflux block having a plurality of detachable reflux vessels corresponding to the reaction vessels. And the vaporized substance in the reaction vessel is condensed in the reflux vessel, whereby the evaporation of the solvent in the reaction vessel can be reduced.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明の反応容器及び還流容器の概略を説明す
るための断面図である。
FIG. 1 is a sectional view schematically illustrating a reaction vessel and a reflux vessel of the present invention.

【図2】本発明の自動合成機の反応部の概略を説明する
ための一部を切り欠いた斜視図である。
FIG. 2 is a partially cutaway perspective view schematically illustrating a reaction section of the automatic synthesizer of the present invention.

【図3】本発明の自動合成機の反応部の概略を説明する
ための還流ブロックの一部を切り欠いた斜視図である。
FIG. 3 is a perspective view, partially cut away, of a reflux block for explaining an outline of a reaction section of the automatic synthesizer of the present invention.

【図4】本発明の自動合成機の反応部の概略を説明する
ための反応ブロックの一部を切り欠いた斜視図である。
FIG. 4 is a perspective view of a reaction block of the automatic synthesizer of the present invention, for explaining the outline of the reaction section, with a part of a reaction block cut away.

【図5】本発明の自動合成機の反応部の断面図である。FIG. 5 is a sectional view of a reaction section of the automatic synthesizer of the present invention.

【図6】本発明の自動合成機の反応部の断面図である。FIG. 6 is a sectional view of a reaction section of the automatic synthesizer of the present invention.

【図7】本発明の自動合成機の反応部の還流ブロックの
上面、及び反応ブロックないし還流ブロック内の熱交換
手段の配置を示す平面図である。
FIG. 7 is a plan view showing an upper surface of a reflux block of a reaction section of the automatic synthesizer of the present invention and an arrangement of a heat exchange means in the reaction block or the reflux block.

【図8】本発明の自動合成機の反応部の他の構成を説明
するための図である。
FIG. 8 is a diagram for explaining another configuration of the reaction section of the automatic synthesizer of the present invention.

【図9】本発明の自動合成機の反応容器の他の構成を説
明するための平面図、及び断面図である。
FIG. 9 is a plan view and a cross-sectional view for explaining another configuration of the reaction vessel of the automatic synthesizer of the present invention.

【図10】本発明の自動合成機の反応容器の他の構成の
空間部分を説明するための透視図である。
FIG. 10 is a perspective view for explaining a space portion of another configuration of the reaction vessel of the automatic synthesizer of the present invention.

【図11】本発明の自動合成機のガス用溝及び凹部を説
明するための斜視図である。
FIG. 11 is a perspective view for explaining gas grooves and concave portions of the automatic synthesizer of the present invention.

【符号の説明】[Explanation of symbols]

1…自動合成機反応部、2…還流容器、3…反応容器、
4…還流ブロック、5反応ブロック…、6…シール材、
7…上蓋、21,55…開口部、22…パッキング、3
1…反応室、32…導出管、33…導出部、34…保守
用押しねじ、35…フィルター、36…接続管、37…
空間部分、41…還流ブロック本体、42,54…熱媒
流路押さえ、43,53…収納部、44…ガス用溝、4
5…溝、46…凹部、48,58…熱媒流路、52…ヒ
ータ押さえ、59…ヒータ、61…凸部。
DESCRIPTION OF SYMBOLS 1 ... Reaction part of an automatic synthesizer, 2 ... Reflux container, 3 ... Reaction container,
4 ... reflux block, 5 reaction block ..., 6 ... sealing material,
7 top lid, 21, 55 opening, 22 packing, 3
DESCRIPTION OF SYMBOLS 1 ... Reaction chamber, 32 ... Outgoing pipe, 33 ... Outgoing part, 34 ... Maintenance screw, 35 ... Filter, 36 ... Connecting pipe, 37 ...
Space portion, 41: reflux block main body, 42, 54: heat medium flow channel holding member, 43, 53: storage portion, 44: gas groove, 4
5 ... groove, 46 ... concave part, 48, 58 ... heat medium flow path, 52 ... heater press, 59 ... heater, 61 ... convex part.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 北村 顕一 神奈川県秦野市堀山下字松葉380−1 株式会社 島津製作所 秦野工場内 (56)参考文献 特表 平8−502482(JP,A) (58)調査した分野(Int.Cl.7,DB名) B01J 19/00 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Kenichi Kitamura 380-1 Matsuba, Horiyamashita, Hadano-shi, Kanagawa Inside the Hadano Plant, Shimadzu Corporation (56) References Special Table 8-82-482482 (JP, A) (58) ) Surveyed field (Int. Cl. 7 , DB name) B01J 19/00

Claims (4)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 化学反応により複数の化合物の同時合成
を可能とする自動合成機において、 複数個の反応容器と、 前記反応容器を個々に着脱可能とする収納部と熱交換手
段を伝熱部材内に有した反応ブロックとを備え、 前記熱交換手段は、収納部内に収納した反応容器の温度
条件の制御を行うことを特徴とする自動合成機。
1. An automatic synthesizer capable of simultaneously synthesizing a plurality of compounds by a chemical reaction, comprising: a plurality of reaction vessels; a storage section for individually detachably attaching the reaction vessels; and a heat exchange means. An automatic synthesizing apparatus, comprising: a reaction block provided therein; and the heat exchange unit controls temperature conditions of the reaction container housed in the housing.
【請求項2】 化学反応により複数の化合物の同時合成
を可能とする自動合成機において、 複数個の反応容器と、 前記反応容器を個々に着脱可能とする収納部と熱交換手
段を伝熱部材内に有した反応ブロックと、 前記反応容器に対応した複数の還流容器を着脱可能に有
する還流ブロックとを備え、 前記反応容器内の気化物質を還流容器内で凝縮させ、反
応容器に戻すことを特徴とする自動合成機。
2. An automatic synthesizer capable of simultaneously synthesizing a plurality of compounds by a chemical reaction, comprising: a plurality of reaction vessels; a storage section capable of individually attaching and detaching the reaction vessels; and a heat exchange means. A reaction block provided therein, and a reflux block having a plurality of detachable reflux containers corresponding to the reaction containers, wherein a vaporized substance in the reaction container is condensed in the reflux container and returned to the reaction container. A special feature of the automatic synthesizer.
【請求項3】 前記反応容器は、反応室と、化合物を導
出する導出管と、反応室の下方側と導出部の上方側とを
接続する接続管とを備え、 前記反応室と導出管は並列して配置し、前記接続管は反
応室と導出管が形成する面に対して傾斜して配置する、
請求項1,又は2記載の自動合成機。
3. The reaction vessel includes a reaction chamber, a discharge pipe for discharging a compound, and a connection pipe connecting a lower side of the reaction chamber and an upper side of the discharge section, wherein the reaction chamber and the discharge pipe are connected to each other. Arranged in parallel, the connecting pipe is arranged inclined with respect to the plane formed by the reaction chamber and the outlet pipe,
The automatic synthesizer according to claim 1.
【請求項4】 前記反応容器を収納するブロックは複数
個の凹部を備え、凹部の底面は一部に反応容器を挿入す
る開口部を有し、凹部はブロック上面に形成されるガス
供給用溝により連結される、請求項1,2,又は3記載
の自動合成機。
4. A block for accommodating the reaction vessel includes a plurality of recesses, a bottom surface of the recess partially having an opening for inserting the reaction vessel, and the recess is a gas supply groove formed on the top surface of the block. The automatic synthesizer according to claim 1, wherein the automatic synthesizer is connected by:
JP10269181A 1997-09-30 1998-09-24 Automatic synthesizer Expired - Fee Related JP3066862B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10269181A JP3066862B2 (en) 1997-09-30 1998-09-24 Automatic synthesizer

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP9-266507 1997-09-30
JP26650797 1997-09-30
JP10269181A JP3066862B2 (en) 1997-09-30 1998-09-24 Automatic synthesizer

Publications (2)

Publication Number Publication Date
JPH11165063A JPH11165063A (en) 1999-06-22
JP3066862B2 true JP3066862B2 (en) 2000-07-17

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4569850B2 (en) * 1998-09-24 2010-10-27 株式会社島津製作所 Automatic synthesizer
US6692708B2 (en) * 2001-04-05 2004-02-17 Symyx Technologies, Inc. Parallel reactor for sampling and conducting in situ flow-through reactions and a method of using same
EP1291075B1 (en) * 2001-09-07 2007-04-11 F. Hoffmann-La Roche Ag Reaction block for parallel synthetic chemistry and vessel therefor
EP1525049B1 (en) * 2002-08-02 2007-07-04 Avantium International B.V. An assembly and method for performing parallel chemical experiments, in particular crystallisation experiments
JP4746857B2 (en) * 2004-09-08 2011-08-10 柴田科学株式会社 Connection adapter
US7794666B2 (en) * 2006-02-07 2010-09-14 Beckman Coulter, Inc. Method and apparatus for controlling reaction temperature in bio-chemical instruments

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