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Ammonium Chloride → 3-(Dimethylphosphoryl)aniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Dimethylphosphoryl-3-nitrobenzene | HCID 190278 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(Dimethylphosphoryl)aniline | HCID 58207781 | 100.1% |
反応手順
To a solution of compound 286 (1.5 g, 7.5 mmol) in methanol (62 ml) and water (12 ml) under nitrogen at room temperature was added ammonium chloride (0.604 g, 11.3 mmol) and iron (1.68 g, 30.1 mmol). The resulting mixture was heated to reflux for 30 min then filtered through celite. The celite pad was rinsed with methanol. The filtrate and washings were combined and concentrated and the residue was purified via Biotage (linear gradient 0-20%, methanol/dichloromethane; 25M column) to afford compound 287 as a yellow solid (1.27 g, 7.51 mmol, quantitative). MS (m/z): 170.1 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759522B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-28bb42a3a65344309b891ef14b6857dd |
| 出典メモ | uspto-grants-2014_06 |