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Hydrochloric Acid → 2-Cyano-2-(3,4-dichloro-5(2H)-oxo-2-furyl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cyanoacetamide | HCID 7898 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Mucochloric Acid | HCID 2771871 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Cyano-2-(3,4-dichloro-5(2H)-oxo-2-furyl)acetamide | HCID 541792 | 17.8% |
反応手順
Mucochloric acid (15.1 g) and 2-cyanoacetamide (7.53 g) were dissolved in methanol (53.6 ml), and 2.5N aqueous sodium hydroxide solution (53.6 ml) was added dropwise with stirring under ice-cooling. The mixture was allowed to warm to room temperature, and further stirred at room temperature for 3 hr. The reaction mixture was poured into 1N hydrochloric acid containing ice water, methanol was evaporated under reduced pressure, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was crystallized from ethanol-diisopropyl ether to give the title compound (3.74 g) as pale-brown crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08481569B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-cf68c47ef71349c1880e6365e5ca62c0 |
| 出典メモ | uspto-grants-2013_07 |