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Pyridine → 4-Bromo-5-nitro-thiophene-2-carbaldehyde oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 4-Bromo-5-nitrothiophene-2-carbaldehyde | HCID 21886281 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Bromo-5-nitro-thiophene-2-carbaldehyde oxime | HCID 73852152 | 88% |
反応手順
Hydroxylamine hydrochloride (85 g, 1.2 mol) was added to a solution of 4-bromo-5-nitro-thiophene-2-carbaldehyde (234 mg, 0.529 mmol, Example 286: step a) in EtOH (7.5 mL, 200 proof—anhydrous):pyridine (100 mL, anhydrous) at rt over 5 min. The reaction mixture was heated to reflux overnight, then cooled to rt. The solvents were removed in vacuo resulting in a solid residue that was washed with water and filtered. The solid was dried overnight under high vacuum to afford the title compound as a yellow solid (225 g, 88%). The solid was used for the next step without further characterization.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07138530B2 |
| 出典データセット | uspto-grants-2006_11 |
| ORD ID | ord-43f2ba13baec47cf9648112fe3674629 |
| 出典メモ | uspto-grants-2006_11 |