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Acetamide, N-[(dimethylamino)methylidene]- → N-[(E)-[(2-bromo-5-fluorophenyl)hydrazinylidene]methyl]acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetamide, N-[(dimethylamino)methylidene]- | HCID 567145 | — |
| 反応物 | (2-Bromo-5-fluorophenyl)hydrazine hydrochloride | HCID 21069774 | — |
| 触媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-[(E)-[(2-bromo-5-fluorophenyl)hydrazinylidene]methyl]acetamide | HCID 136094110 | 72.2% |
反応手順
Alternatively, to a mixture of (2-bromo-5-fluoro-phenyl)-hydrazine hydrochloride (5.9 g, 28.8 mmol) and N-((dimethylamino)methylene)acetamide (3.30 g, 28.8 mmol) in THF (30 mL) was added 5 drops of HOAc, and the mixture stirred at room temperature under nitrogen for 15 min. The mixture was concentrated in vacuo, and the residue suspended in a mixture of ether (50 mL) and hexanes (50 mL) and the resulting precipitate collected and air-dried to provide 5.7 g of the title compound as an off-white powder. A second crop gave an additional 0.3 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08039458B2 |
| 出典データセット | uspto-grants-2011_10 |
| ORD ID | ord-6363612bd71b49dbb79a559ffe5ae706 |
| 出典メモ | uspto-grants-2011_10 |