関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Bromobenzenethiol | HCID 80598 | — |
| 反応物 | 2-Chloro-5-nitrobenzenesulphinic acid | HCID 111523 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(2-Bromo-phenylsulfanyl)-5-nitro-benzenesulfinic acid | HCID 59797437 | — |
反応手順
To a solution of NaOH (80.18 g, 2.004 mol) in water (600 ml sonicated and degassed) was added 2-bromothiophenol (108.23 ml, 1.002 mol) and 2-chloro-5-nitro-benzenesulfinic acid (222.11 g, 1.002 mol). The mixture was stirred and heated at 125° C. for 19 hours. The reaction was cooled down at 0° C., and concentrated HCl added dropwise from a dropping funnel while stirring until pH<1. The precipitate formed was filtered, dried in a desiccators overnight and was used without any further purification (417.77 g). m/z (LC-MS, ESP), RT=3.51 min, (M−−1)=372-374, (1:1, bromine isotope ratio present).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07429660B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-10fa31c5cc2749d2a1fbbb1cd161dbd5 |
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| 出典メモ | uspto-grants-2008_09 |
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