関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chloral Hydrate | HCID 2707 | — |
| 反応物 | P-Anisidine | HCID 7732 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sodium Sulfate | HCID 24436 | — |
| 生成物 | 4-Methoxyisonitrosoacetanilide | HCID 6710791 | 85.2% |
反応手順
Chloral hydrate (9.6 g) was dissolved in 200 mL of water containing 83 g of sodium sulfate. The solution was warmed to 60° C., a solution of 11.4 g of hydroxylamine hydrochloride in 50 mL of water was added and the mixture was held at 60° C. In a separate flask, 6.4 g of 4-anisidine and 4.3 mL of concentrated hydrochloric acid in 80 mL of water was warmed to 80° C. The first solution was added to the second and the mixture refluxed for 2 minutes after which it was cooled slowly to room temperature and then cooled in an ice bath. The tan precipitate was collected by vacuum filtration, washed with water and dried under vacuum to give 8.6 g (85% yield) of N-(2-hydroximino-acetyl)anisidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06855730B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-6aec756dbaea426a847093dad6f4cd85 |
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| 出典メモ | uspto-grants-2005_02 |
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