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Hydroxylamine → 5-Hydroxy-2-pyridinecarboxaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxylamine | HCID 787 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 5-Hydroxy-2-pyridinecarboxaldehyde | HCID 278389 | 30% |
反応手順
N-[5-(N',N'-Dimethylcarbamoyl)hydroxy-2-pyridine methylene] hydroxylamine. Dimethylcarbamoyl chloride (5.2 mL, 57 mmol) was added to a solution of N-(5-hydroxy-2-pyridinemethylene) hydroxylamine (6.53 g, 47 mmol) in 40 mL of pyridine. It was stirred at room temperature overnight and then the solvent was removed in vacuo, leaving a light green paste. The paste was dissolved in a minimum quantity of acetone and then triturated with ethyl acetate and placed in the freezer overnight. Glassy needles formed and were filtered and washed with ethyl acetate to yield 3.0 g of pure product (30%), m.p. 134°-135° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05714615 |
| 出典データセット | uspto-grants-1998_02 |
| ORD ID | ord-143cf03b4ad742c593059d8405a026ef |
| 出典メモ | uspto-grants-1998_02 |