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Cyanuric chloride → 1-[(4,6-Dichloro-1,3,5-triazin-2-yl)amino]imidazolidine-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyanuric chloride | HCID 7954 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-Aminohydantoin hydrochloride | HCID 12472963 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-[(4,6-Dichloro-1,3,5-triazin-2-yl)amino]imidazolidine-2,4-dione | HCID 86698065 | 107.2% |
反応手順
An ice-cold suspension of 1-aminohydantoin hydrochloride (457 mg, 3.0 mmol), cyanuric chloride (500 mg, 2.73 mmol) and sodium bicarbonate (505 mg, 6 mmol) in acetonitrile (5 mL) was stirred under an atmosphere of nitrogen for 2 h and then stirred at room temperature for 20 h. The reaction mixture was evaporated to dryness under reduced pressure and the residue was extracted with ethyl acetate and the ethyl acetate was separated and dried (MgSO4). The crude product (770 mg) gave a single spot on thin layer chromatography [silica; CH2Cl2/MeOH (10:1)] and was used in the next step without further purification. NMR (CD3CN): δ=4.11 (s, 2H); 8.71 (s, 1H); 8.85 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835629B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-1eddf919437649cab3c98bfcaf8416ae |
| 出典メモ | uspto-grants-2014_09 |