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Ammonium Chloride → 5-Bromo-3-tert-butyl-2-methoxyaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 5-Bromo-1-tert-butyl-2-methoxy-3-nitrobenzene | HCID 22930147 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Methanol--water (1/1) | HCID 22242641 | — |
| 生成物 | 5-Bromo-3-tert-butyl-2-methoxyaniline | HCID 22930155 | 90.2% |
反応手順
Ammonium chloride (38 g) was added to a solution of 4-bromo-2-(tert-butyl)-6-nitrophenyl methyl ether (20.6 g) in methanol-water (140 ml-140 ml) and iron (20 g) was gradually added while heating to reflux. The mixture was heated to reflux for 2 hours and then the reaction mixture was filtered through celite. The filtrate was concentrated under reduced pressure, ethyl acetate was added to the residue and the mixture was washed 3 times with brine. The organic layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to yield a crude product of the title compound (16.65 g) as a brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07244730B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-31d009973dda471c80f221d5e1704f13 |
| 出典メモ | uspto-grants-2007_07 |