化工社化工社 化学情報印刷レポート · 研究参考用
2-Bromo-4-methylaniline → 2-Amino-5-methylbenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Bromo-4-methylaniline | HCID 11422 | — |
| 反応物 | HCID 178418546 | HCID 178418546 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 2-Amino-5-methylbenzonitrile | HCID 242778 | 60% |
反応手順
Combine 2-bromo-4-methyl-phenylamine (8.00 g, 43.0 mmol), CuCN (4.62 g, 51.6 mmol), and NMP (30.0 ml) and stir at reflux. After 75 minutes, cool to ambient temperature, pour the mixture onto ice chips and stir for 1 hour. Remove the resulting precipitate by vacuum filtration. Dissolve the precipitate in NH4OH and extract with dichloromethane. Combine, wash (brine), dry (sodium sulfate), and reduce the extracts to residue. Purify the residue on silica gel using dichloromethane/hexanes (75:25) to give 3.39 g (60%) of an orange solid: mass spectrum (ion spray): m/z=133.1 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07384934B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-04bb8768009749168397a3561c82c357 |
| 出典メモ | uspto-grants-2008_06 |