関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isatoic Anhydride | HCID 8359 | — |
| 反応物 | 2-Hydrazinopyridine | HCID 78645 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-amino-benzoic acid N'-pyridin-2-yl-hydrazide | HCID 68533562 | 546.1% |
反応手順
A mixture of isatoic anhydride (3.51 g, 2.15 mmol) and 2-hydrazinopyridine (2.40 g, 2.20 mmol) in 35 ml of EtOH was refluxed for 17 hours. After refluxing for 15 minutes, the suspension turned into a brown solution and gas evolution was observed. At the end of the 17 hour period, the reaction mixture was cooled to room temperature and the brown solution was concentrated on a rotary evaporator. The residue was chromatographed on silica gel with 65% EtOAc in hexanes. The fractions containing the product were collected and concentrated. The solid was triturated with ether (100 ml) for 15 minutes and collected by filtration. It was air-dried to give 2.68 g of 2-amino-benzoic acid N′-pyridin-2-yl-hydrazide (Intermediate 9) as a white solid. MS (APCI): 229 (M+1, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07423054B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-8628a3cc9ef94a3f9cd200bd63018a30 |
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| 出典メモ | uspto-grants-2008_09 |
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