関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | O-Phenylenediamine | HCID 7243 | — |
| 反応物 | 5-Bromo-2-chlorobenzoic acid | HCID 33127 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 2-(5-Bromo-2-chlorophenyl)-1H-benzo[d]imidazole | HCID 43379066 | — |
反応手順
Into a one necked round bottomed flask equipped with a magnetic stirrer, 5-bromo-2-chlorobenzoic acid (70.0 g, 297.3 mmol), o-phenylenediamine (64.3 g, 594.6 mmol) and methansulfonic acid (140 mL) were placed and heated to 170° C. in order to melt the solids. The system was stirred 5 h at this temperature, then left to come rt. The blue solid was treated with NaOH 35% (200 mL) obtaining a violet suspension (pH 5) that was filtered and washed with NaOH 0.5 M (2 L) and H2O (2 L). The product was dried under vacuum (60° C.), to give 61.6 g of a pure violet solid. (67%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08592463B2 |
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| 出典データセット | uspto-grants-2013_11 |
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| ORD ID | ord-204b368ab2f44b2e9f22f4cf0bde3f4a |
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| 出典メモ | uspto-grants-2013_11 |
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