JP4753367B2 - 有機合成反応装置 - Google Patents
有機合成反応装置 Download PDFInfo
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- 238000003786 synthesis reaction Methods 0.000 title claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 146
- 239000003153 chemical reaction reagent Substances 0.000 claims description 121
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- 238000001514 detection method Methods 0.000 claims description 19
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
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- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 3
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical compound FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 description 3
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- 230000015572 biosynthetic process Effects 0.000 description 2
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- 238000004435 EPR spectroscopy Methods 0.000 description 1
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- 238000012916 structural analysis Methods 0.000 description 1
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- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
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- B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
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- B01F33/30—Micromixers
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- G01R33/30—Sample handling arrangements, e.g. sample cells, spinning mechanisms
- G01R33/302—Miniaturized sample handling arrangements for sampling small quantities, e.g. flow-through microfluidic NMR chips
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
- G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
- G01R33/30—Sample handling arrangements, e.g. sample cells, spinning mechanisms
- G01R33/307—Sample handling arrangements, e.g. sample cells, spinning mechanisms specially adapted for moving the sample relative to the MR system, e.g. spinning mechanisms, flow cells or means for positioning the sample inside a spectrometer
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
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Description
図8に示すように、マイクロチップの流路上に円形の液溜めを作製し、それにマイクロコイルを近接させ、微量試料を測定するという研究が論文レベルで報告されている。マイクロチップ専用のマイクロコイルやプローブの研究が行なわれている段階である。合成に応用した例はほとんどない。
スタティックミキサーなどを用いて、反応試薬を混合・反応させ、反応液をラインを介してフローNMR用のプローブに導いてNMR測定を行なう。実用化レベルの研究である。この実験にはフローNMRプローブが必要であり、反応部からNMRマグネット内の高周波磁場照射位置までの距離が長くなるという欠点がある。
図9に示すように、マイクロチップ作製時に、ナノエレクトロスプレーノズルをチップと一体型で作製する。ノズルに高電圧を印加することで、質量分析が可能となる。合成化学よりバイオ分野への応用例が多い。
(1)一体型であり、部分交換ができないので、流路や配管接続部などの閉塞によって全体を交換しなければならず、ガラス製などではランニングコストがかかる。
(2)コネクター部の材質からの溶出物やデッドボリュームが問題となる。
(3)生成物のオンライン検出においては、検出器は分光光度計類に制限される。
(4)生成物の分析装置による構造解析には、通常、オフライン的な試料導入を要する。
という問題があった。
(1)専用のNMRプローブを設計開発する必要があり、莫大な初期投資が必要である。
(2)マイクロチップのデザインがNMR専用であり、他の検出器にそのまま接続するのは困難である。
という問題があった。
(1)専用のフロープローブを設計開発する必要があり、莫大な初期投資が必要である。
(2)反応部をプローブ内に持ち込むことは困難であり、通常、マグネットの外に反応部を配置するため、反応から検出までにタイムラグがある。
という問題があった。
(1)化学合成に応用されている例は少ない。
(2)マイクロチップのデザインがMS専用であり、他の検出器にそのまま接続するのは困難である。
という問題があった。
該導入部と切り離し可能に接続され、該導入部から導入された試薬または反応液を更に別の試薬と混合し反応させる反応部と
から成り、流体を微細空間で混合し多段階反応させる柱状体の有機合成反応装置であって、
前記導入部は、
前記柱状体の一端の側面で試薬を導入する試薬導入孔を有し試薬を外部から前記反応部に導入する導入流路と、
前記側面と同一の側面で反応液を排出する反応液排出孔を有し前記反応部から排出される反応液を外部に排出する排出流路と
を一方は上面側に他方は下面側に備え、
前記反応部は、
前記導入流路と連通し、該導入流路から送られてくる複数の試薬を混合し反応させる反応流路と、
前記反応流路と連通し、前記反応流路で生成する反応液を分析する分析装置と組み合わせて使用するための検出部流路と、
前記上面側と下面側とを貫通して前記検出部流路と前記排出流路に連通し、前記反応液を前記検出部流路から前記導入部に戻す反応液排出流路と
を備えていることを特徴としている。
複数の試薬を複数の流路から導入し、必要があればそれを混合し反応させる導入部と、
該導入部と切り離し可能に接続され、該導入部から導入された試薬または反応液を更に別の試薬と混合し反応させる反応部と
から成り、流体を微細空間で混合し多段階反応させる柱状体の有機合成反応装置であって、
前記導入部は、
前記柱状体の一端の側面で試薬を導入する試薬導入孔を有し試薬を外部から前記反応部に導入する導入流路と、
前記側面と同一の側面で反応液を排出する反応液排出孔を有し前記反応部から排出される反応液を外部に排出する排出流路と
を一方は上面側に他方は下面側に備え、
前記反応部は、
前記導入流路と連通し、該導入流路から送られてくる複数の試薬を混合し反応させる反応流路と、
前記反応流路と連通し、前記反応流路で生成する反応液を分析する分析装置と組み合わせて使用するための検出部流路と、
前記上面側と下面側とを貫通して前記検出部流路と前記排出流路に連通し、前記反応液を前記検出部流路から前記導入部に戻す反応液排出流路と
を備えているので、
多くの分析装置と組み合わせて使用できるようなマイクロチップタイプの有機合成反応装置を提供することができる。
Claims (3)
- 複数の試薬を複数の流路から導入し、必要があればそれを混合し反応させる導入部と、
該導入部と切り離し可能に接続され、該導入部から導入された試薬または反応液を更に別の試薬と混合し反応させる反応部と
から成り、流体を微細空間で混合し多段階反応させる柱状体の有機合成反応装置であって、
前記導入部は、
前記柱状体の一端の側面で試薬を導入する試薬導入孔を有し試薬を外部から前記反応部に導入する導入流路と、
前記側面と同一の側面で反応液を排出する反応液排出孔を有し前記反応部から排出される反応液を外部に排出する排出流路と
を一方は上面側に他方は下面側に備え、
前記反応部は、
前記導入流路と連通し、該導入流路から送られてくる複数の試薬を混合し反応させる反応流路と、
前記反応流路と連通し、前記反応流路で生成する反応液を分析する分析装置と組み合わせて使用するための検出部流路と、
前記上面側と下面側とを貫通して前記検出部流路と前記排出流路に連通し、前記反応液を前記検出部流路から前記導入部に戻す反応液排出流路と
を備えていることを特徴とする有機合成反応装置。 - 前記導入部は、耐薬品性樹脂の基板に微小流路を配設したマイクロチップ、前記反応部は、ガラスまたは石英の基板に微小流路を配設したマイクロチップであることを特徴とする請求項1記載の有機合成反応装置。
- 前記分析装置は、NMR、ESR、および熱レンズ顕微鏡のうちの少なくとも1つであることを特徴とする請求項1または2記載の有機合成反応装置。
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JP2006110573A JP4753367B2 (ja) | 2005-11-25 | 2006-04-13 | 有機合成反応装置 |
US11/603,948 US20070148054A1 (en) | 2005-11-25 | 2006-11-22 | Apparatus for organic synthesis and reactions |
EP06256020A EP1790411A1 (en) | 2005-11-25 | 2006-11-24 | Apparatus for organic synthesis and reactions |
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JP2005339570 | 2005-11-25 | ||
JP2006110573A JP4753367B2 (ja) | 2005-11-25 | 2006-04-13 | 有機合成反応装置 |
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JP2007171155A JP2007171155A (ja) | 2007-07-05 |
JP4753367B2 true JP4753367B2 (ja) | 2011-08-24 |
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JP4933352B2 (ja) * | 2006-07-24 | 2012-05-16 | 株式会社 Jeol Resonance | Nmr装置 |
CN102341153B (zh) * | 2009-03-06 | 2014-07-02 | 沃特世科技公司 | 至微流体基底的电喷雾接口 |
EP2407796B1 (en) | 2010-07-12 | 2013-03-06 | Bruker BioSpin Corporation | NMR flow cell |
CA3033346A1 (en) * | 2016-08-09 | 2018-02-15 | Beth Israel Deaconess Medical Center, Inc. | System and method for microfluidic parahydrogen induced polarization hyperpolarizer for magnetic resonance imaging (mri) and nuclear magnetic resonance (nmr) applications |
US20220276327A1 (en) * | 2019-08-06 | 2022-09-01 | National University Corporation Hokkaido University | Polarization-transfer apparatus, and microfluidic device |
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JPS6120523Y2 (ja) * | 1980-10-24 | 1986-06-20 | ||
EP0637997B1 (en) * | 1992-05-01 | 1998-07-01 | Trustees Of The University Of Pennsylvania | Analysis based on flow restriction |
US5498392A (en) * | 1992-05-01 | 1996-03-12 | Trustees Of The University Of Pennsylvania | Mesoscale polynucleotide amplification device and method |
JP2948069B2 (ja) * | 1993-09-20 | 1999-09-13 | 株式会社日立製作所 | 化学分析装置 |
US5580523A (en) * | 1994-04-01 | 1996-12-03 | Bard; Allen J. | Integrated chemical synthesizers |
DE19854096A1 (de) * | 1998-11-24 | 2000-05-25 | Merck Patent Gmbh | Anschlußträger für plattenförmige Mikrokomponenten |
DE19945832A1 (de) * | 1999-09-24 | 2001-04-05 | Karlsruhe Forschzent | Modular aufgebauter Mikroreaktor |
JP2001194373A (ja) * | 2000-01-06 | 2001-07-19 | Olympus Optical Co Ltd | 超小型化学操作装置 |
DE10036633B4 (de) * | 2000-07-27 | 2005-03-10 | Hte Ag The High Throughput Exp | Anordnung in modularer Bauweise und Verfahren zur paralellen Testung einer Mehrzahl von Bausteinen einer Materialbibliothek |
US6827095B2 (en) * | 2000-10-12 | 2004-12-07 | Nanostream, Inc. | Modular microfluidic systems |
US6653625B2 (en) * | 2001-03-19 | 2003-11-25 | Gyros Ab | Microfluidic system (MS) |
US7129091B2 (en) * | 2002-05-09 | 2006-10-31 | University Of Chicago | Device and method for pressure-driven plug transport and reaction |
US20050169815A1 (en) * | 2002-05-13 | 2005-08-04 | Avantium International B.V. | System for chemical experiments |
US20030224531A1 (en) * | 2002-05-29 | 2003-12-04 | Brennen Reid A. | Microplate with an integrated microfluidic system for parallel processing minute volumes of fluids |
US7402719B2 (en) * | 2002-06-13 | 2008-07-22 | Velocys | Catalytic oxidative dehydrogenation, and microchannel reactors for catalytic oxidative dehydrogenation |
JP2004138583A (ja) * | 2002-10-21 | 2004-05-13 | Sumitomo Bakelite Co Ltd | 細胞機能測定用マイクロチップ |
EP1637221A4 (en) * | 2003-03-19 | 2008-01-23 | Tosoh Corp | BODY WITH MICRO CHANNEL STRUCTURE |
FR2865806B1 (fr) * | 2004-01-30 | 2007-02-02 | Commissariat Energie Atomique | Laboratoire sur puce comprenant un reseau micro-fluidique et un nez d'electronebulisation coplanaires |
US20060148089A1 (en) * | 2004-12-30 | 2006-07-06 | Symyx Technologies, Inc. | Small scale ideal kinetic reactor to evaluate full size industrial catalysts |
JP4933352B2 (ja) * | 2006-07-24 | 2012-05-16 | 株式会社 Jeol Resonance | Nmr装置 |
-
2006
- 2006-04-13 JP JP2006110573A patent/JP4753367B2/ja active Active
- 2006-11-22 US US11/603,948 patent/US20070148054A1/en not_active Abandoned
- 2006-11-24 EP EP06256020A patent/EP1790411A1/en not_active Withdrawn
Also Published As
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US20070148054A1 (en) | 2007-06-28 |
EP1790411A1 (en) | 2007-05-30 |
JP2007171155A (ja) | 2007-07-05 |
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