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 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 4-Bromo-3-methoxyaniline | HCID 7018254 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (2E)-N-(4-bromo-3-methoxyphenyl)-2-hydroxyiminoacetamide | HCID 14595057 | 111.2% |
反応手順
A mixture of 4-bromo-3-(methyloxy)aniline (50 g, 247 mmol), HCl (100 mL) and dioxane (150 mL) in H2O (500 mL) was stirred at 50° C. 2,2,2-Trichloro-1,1-ethanediol (81.7 g, 494 mmol), Na2SO4 (526 g, 3705 mmol) and H2O (1 L) were added to the mixture followed by NH2OH.HCl (103 g, 1482 mmol in 100 mL of H2O). The mixture was stirred at 80° C. for 1 h, cooled to room temperature, filtered and washed with H2O to yield (2E)-N-[4-bromo-3-(methyloxy)phenyl]-2-(hydroxyimino)ethanamide (75 g) as a yellow solid. MS (m/z) 273 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08658636B2 |
|---|
| 出典データセット | uspto-grants-2014_02 |
|---|
| ORD ID | ord-cd35bce504984b59999165bdf887ceac |
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| 出典メモ | uspto-grants-2014_02 |
|---|
