JP2011506072A - 誘導的に加熱された熱媒体を用いて化学反応を行う方法 - Google Patents
誘導的に加熱された熱媒体を用いて化学反応を行う方法 Download PDFInfo
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Abstract
Description
誘導性:134マイクロヘンリー、スプールの屈曲数:=2〜16、断面積=2.8mm2(断面積は、誘導子中の導線の数とその直径に由来する)。管型リアクターを受けるためのギャップの直径は、12mmであった。全ての実験において、誘導子を25kHzの周波数で稼働させた。
実験を、25kHzの周波数、EW5ユニット(出力5ワット)、乾燥粉体(流れない)で行った。それぞれの加熱時間は10分間であり、温度を高温計により測定した。以下の熱媒体を試験した:
a)MagSilica(登録商標)58/85:Evonik(以前はDegussa)製、
b)マンガンフェライト粉末:SusTech GmbH(ダルムシュタット)製、
c)Bayferrox(登録商標)318M:合成α−Fe3O4:Harald Scholz & Co. GmbH製
d)マンガン−亜鉛−フェライト、オレイン酸による表面被覆、フェライト含量51.7重量%:SusTech GmbH(ダルムシュタット)製。
反応のために、所望の加熱を誘導子により得るために、前述の物質3.3gをリアクターに充填した。
物質の完全な混合を確保するために、触媒の調製に攪拌機を使用した。従来の濾紙は、細孔が急速に塞がれてしまうため、洗浄に不適当であることがわかった。したがって、固形物を、各洗浄工程で遠心分離した。磁性特性または磁性分離を、市販の磁石で試験した。
表2:Heck−Mizorokiカップリング反応、1mmolハロゲン化アリール、3当量スチレン、3当量n−Bu3N、2.8mol%触媒7、反応時間各1時間、流速2mL/min、PWM=325‰
2mL/min、反応時間各1時間、:0.5mmolハロゲン化アリール、1.5当量ボロン酸、2.4当量CsF、PWM750‰
a1mol%、b2.8mol%
桂皮酸エチル(59)から桂皮酸メチル(60)へのエステル交換。この実験は、下記の文献(K. Jansson, T. Fristedt, A. Olsson, B. Svensson, S. Joensson, J. Org. Chem.、2006年、71、1658-1667)の方法により行った。エステル交換平衡を所望の生成物へ移行するため、過剰のナトリウムメタノレートを使用した。誘導的加熱(流速:2mL/min、PWM=240‰)により、25分後に93%の生成物が単離された。
(prom=PWM(‰)、下記の生成物の式の数字(%)は生成物の収率を表す。)
Claims (14)
- リアクター内で、少なくとも1つの第1反応性物質を含む反応媒体を加熱し、第1反応性物質中、または第1と第2の反応性物質の間で化学結合を形成または修飾することにより目的化合物を製造するための化学反応を行う方法であって、電磁誘導により加熱することができ、かつリアクターの内側にあり反応媒体により囲まれている固形熱媒体と反応媒体を接触させ、前記熱媒体を誘導子を用いて電磁誘導により加熱し、目的化合物を第1反応性物質からまたは第1反応性物質と第2反応性物質とから形成し、前記目的化合物を電熱媒体から分離する方法。
- 熱媒体が導電性および/または磁化性固体の粒子から選択され、該粒子の平均粒度が1〜1000nmである請求項1に記載の方法。
- 熱媒体が磁化性固体の粒子から選択され、各粒子が非磁性物質によりカプセル化された少なくとも1つの磁化性物質のコアを含んでなる請求項2に記載の方法。
- 熱媒体が磁化性固体の粒子から選択され、これらが電磁誘導により加熱できないさらなる粒子との混合物中に存在している、請求項2または3に記載の方法。
- 固形熱媒体が、化学反応に対する触媒活性物質により表面被覆されている、請求項1〜4のいずれかに記載の方法。
- 化学反応をバッチ式で行い、反応中、反応媒体および固形熱媒体が互いに移動し合う、請求項1〜5のいずれかに記載の方法。
- 反応媒体が反応槽中に熱媒体の粒子とともに存在し、反応媒体に誘導子として配置された可動素子により反応媒体を移動させることにより熱媒体の粒子を加熱する、請求項6に記載の方法。
- 少なくとも部分的に固形熱媒体が充填されることにより、電磁誘導によって加熱し得る少なくとも1つの加熱領域を有するフロー型リアクターで化学反応を行い、反応媒体がフロー型リアクター内を流れ、誘導子がリアクター外部に配置されている、請求項1〜5のいずれかに記載の方法。
- 反応媒体と熱媒体との総接触時間が1秒〜2時間の範囲になるような速度で、反応媒体がフロー型リアクター内を1回または複数回流れる、請求項8に記載の方法。
- リアクターが圧力リアクターとして構成され、化学反応を大気圧より高い圧力で、好ましくは少なくとも1.5barの圧力下で行う、請求項1〜9のいずれかに記載の方法。
- 反応媒体がリアクター内で液体として存在する、請求項1〜10のいずれかに記載の方法。
- 誘導子が、1〜100kHzの範囲の、好ましくは10〜80kHzの範囲の周波数の交番磁場を生じる、請求項1〜11のいずれかに記載の方法。
- 熱媒体が強磁性体であって、40〜250℃の範囲のキュリー温度を示し、かつ、キュリー温度が選択された反応温度から20℃より大きく異ならないように熱媒体を選択する、請求項1〜12のいずれかに記載の方法。
- 化学反応において、化学結合を2つの炭素原子の間に、または炭素原子と原子X〔Xは、H、B、O、N、S、P、Si、Ge、Sn、Pb、As、Sb、Biおよびハロゲンから選択される〕との間に形成する、請求項1〜13のいずれかに記載の方法。
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Also Published As
Publication number | Publication date |
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ES2367467T3 (es) | 2011-11-03 |
EP2219778B1 (de) | 2011-07-13 |
US8871964B2 (en) | 2014-10-28 |
DE102007059967A1 (de) | 2009-06-18 |
WO2009074373A1 (de) | 2009-06-18 |
US20100249404A1 (en) | 2010-09-30 |
KR20100098387A (ko) | 2010-09-06 |
EP2219778A1 (de) | 2010-08-25 |
ATE516077T1 (de) | 2011-07-15 |
JP5587200B2 (ja) | 2014-09-10 |
CN101896263A (zh) | 2010-11-24 |
US20120202994A1 (en) | 2012-08-09 |
CN101896263B (zh) | 2014-09-03 |
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