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Methyl iodide → 4-Methoxy-N-methyl-2-nitrobenzenamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Methoxy-2-nitroaniline | HCID 66793 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 4-Methoxy-N-methyl-2-nitrobenzenamine | HCID 3554313 | — |
反応手順
To 4-methoxy-2-nitroaniline (10 mmol, 1.68 g) in 20 mL of DMF was added NaH (12 mmol, 480 mg of a 60% dispersion in mineral oil) (exothermic, H2 evolution), affording a deep red slurry. After 15 min MeI (20 mmol, 1.2 mL) was added (exothermic). After 30 min the reaction was poured into a solution of brine and NaHCO3, resulting in formation of a bright orange precipitate. The slurry was filtered and the filter cake was washed with H2O. The solid was dried under reduced pressure, affording a bright orange solid. HPLC A: 1.77 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07563815B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-0681ef451e024f8f8ef93e82d1e8a705 |
| 出典メモ | uspto-grants-2009_07 |