化工社化工社 化学情報印刷レポート · 研究参考用
1-Bromo-4-fluoro-2-methyl-5-nitrobenzene → 5-Bromo-2-fluoro-4-methylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Bromo-4-fluoro-2-methyl-5-nitrobenzene | HCID 10036983 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-Bromo-2-fluoro-4-methylaniline | HCID 46739114 | 63.2% |
反応手順
Combine crude 1-bromo-4-fluoro-2-methyl-5-nitrobenzene (32.4 g, 138 mmol), ethanol (100 mL) and Raney Nickel (1.00 g, 17.04 mmol) in a shaker flask. Charge the flask with hydrogen (275 kPa) and agitate until the absorption of hydrogen ceases. De-pressurize the reaction vessel, remove the catalyst by filtration, and evaporate the filtrate to dryness. Add MTBE, then filter again and evaporate the filtrate. Stir residue in hexanes. Collect the solids by filtration, wash with cold hexanes and dry in vacuo to provide the title compound (17.8 g, 63% yield) as a dark solid. MS (m/z): 204.0 (M+1)/206.0 (M+3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09334267B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-ee685ee613564d3fa6d76b9da194d191 |
| 出典メモ | uspto-grants-2016_05 |