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Chloral → Acetamide, 2-(hydroxyimino)-N-phenyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloral | HCID 6407 | — |
| 反応物 | 3,5-Dichloroaniline | HCID 12281 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Acetamide, 2-(hydroxyimino)-N-phenyl- | HCID 6861488 | — |
反応手順
To a solution of trichloroacetaldehyde monohydate (13.25 g, 1.3 eq) in H2O (150 mL) was successively added sodium sulfate (17.55 g, 4.0 eq), a hot solution (ca. 80° C.) of 3,5-dichloroaniline (10.0 g, 61.5 mmol) in H2O (50 mL) and 37% HCl (6.1 mL), and a solution of hydroxylamine hydrochloride (16.3 g, 3.8 eq) in H2O (75 mL) with rapid stirring. Once the addition was completed the reaction mixture was heated at reflux for 2 minutes and then allowed to cool to room temperature. The resulting light brown precipitate was filtered, washed with H2O (200 mL) and then dried to yield the crude isonitrosoacetanilide (20.13 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06576656B1 |
| 出典データセット | uspto-grants-2003_06 |
| ORD ID | ord-62e3b4db55134910b92355b50077dc92 |
| 出典メモ | uspto-grants-2003_06 |