関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chloral Hydrate | HCID 2707 | — |
| 反応物 | 3-Bromoaniline | HCID 11562 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Acetamide, N-(3-bromophenyl)-2-(hydroxyimino)- | HCID 6739944 | 85% |
反応手順
To a 3000 mL round bottom flask, 3-bromoaniline (50 g, 0.2907 mol), water (1500 mL), chloral hydrate (57.7 g, 0.3488 mol), hydroxylamine hydrochloride (64.6 g, 0.9302 mol) and sodium sulphate (250 g) were added. To this reaction mixture was slowly added concentrated HCl (76 mL). The reaction mixture was stirred at 90° C. for 2 hours. The white precipitate was formed and was collected by filtration. The white solid was dried to provide the title compound [60 g, 85%]. 1H NMR (300 MHz, DMSO-d6): δ 12.28 (s, 1H), 10.38 (s, 1H), 8.03 (t, J=1.5 Hz, 1H), 7.62-7.65 (m, 2H), 7.29-7.31 (m, 2H). LC-MS (ESI): Calculated mass: 242.0; Observed mass [M+H]+: 243.0 (RT: 0.17 min).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09145411B2 |
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| 出典データセット | uspto-grants-2015_09 |
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| ORD ID | ord-0cfd40d6645c485fb4aa9b15bbd9fdcf |
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| 出典メモ | uspto-grants-2015_09 |
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