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2,2,2-Trifluoroethylhydrazine → 4,5-Dichloro-2-(2,2,2-trifluoroethyl)-3(2H)-pyridazinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,2,2-Trifluoroethylhydrazine | HCID 78740 | — |
| 反応物 | Mucochloric Acid | HCID 2771871 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4,5-Dichloro-2-(2,2,2-trifluoroethyl)-3(2H)-pyridazinone | HCID 13881556 | — |
反応手順
2,2,2-Trifluoroethylhydrazine (70% solution in water, 35.0 g, 0.307 mol) was treated with mucochloric acid (51.88 g, 0.307 mol) in ethanol (300 mL) and refluxed for 5 hours. The solvent was concentrated in vacuo. The crystals obtained were washed with water and air dried (yield: 50 g; 67.5%). 1H NMR (300 MHz, CDCl3) δ 4.8 (q, J=9 Hz, 2H), 7.85 (s, 1H). MS (DCl-NH3) m/z 264 (M+NH4)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06307047B1 |
| 出典データセット | uspto-grants-2001_10 |
| ORD ID | ord-b275da0cabc342c7b5e85ec7bdd06e4d |
| 出典メモ | uspto-grants-2001_10 |